#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:00:21 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223912 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/04/7700498.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7700498
loop_
_publ_author_name
'Mrózek, Ondřej'
'Dostál, Libor'
'Císařová, Ivana'
'Honzíček, Jan'
'Vinklárek, Jaromír'
_publ_section_title
;
 Propene complexes of molybdenum and tungsten stabilized by intramolecular
 coordination of the 1-(quinol-8-yl)indenyl ligand.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12210
_journal_page_last               12218
_journal_paper_doi               10.1039/c9dt02229e
_journal_volume                  48
_journal_year                    2019
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         '2(C22 H18 Mo N O2 S),2(B F4),C H2 Cl2'
_chemical_formula_sum            'C45 H38 B2 Cl2 F8 Mo2 N2 O4 S2'
_chemical_formula_weight         1171.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-06 deposited with the CCDC.    2019-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.503(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5014(7)
_cell_length_b                   11.0265(6)
_cell_length_c                   14.7195(7)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5376
_cell_measurement_theta_min      2.3574
_cell_volume                     2256.7(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.10'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_min         2.344
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0284P)²+2.8869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4529
_reflns_number_total             5192
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02229e2.cif
_cod_data_source_block           jv190319mo1_vinklarek
_cod_depositor_comments
'Adding full bibliography for 7700495--7700499.cif.'
_cod_database_code               7700498
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.764
_shelx_estimated_absorpt_t_max   0.928
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mo1 Mo 0.79407(2) 0.24778(2) 0.33452(2) 0.01357(6) Uani 1 1 d . . .
N1 N 0.64363(11) 0.19438(16) 0.33258(11) 0.0185(3) Uani 1 1 d . . .
C1 C 0.79766(13) 0.04483(17) 0.37808(13) 0.0158(4) Uani 1 1 d . . .
C2 C 0.82333(14) 0.05545(18) 0.29141(14) 0.0178(4) Uani 1 1 d . . .
H2 H 0.788538 0.022811 0.231798 0.021 Uiso 1 1 calc R U .
C3 C 0.90966(13) 0.12315(18) 0.31014(14) 0.0168(4) Uani 1 1 d . . .
H3 H 0.940439 0.148908 0.264459 0.020 Uiso 1 1 calc R U .
C4 C 0.94299(13) 0.14637(17) 0.41141(13) 0.0155(4) Uani 1 1 d . . .
C5 C 0.87335(13) 0.09652(17) 0.45297(13) 0.0144(4) Uani 1 1 d . . .
C6 C 0.88852(13) 0.09827(18) 0.55253(13) 0.0170(4) Uani 1 1 d . . .
H6 H 0.842154 0.065780 0.580231 0.020 Uiso 1 1 calc R U .
C7 C 0.97193(14) 0.14820(19) 0.60707(14) 0.0195(4) Uani 1 1 d . . .
H7 H 0.984337 0.148625 0.674010 0.023 Uiso 1 1 calc R U .
C8 C 1.04098(13) 0.19980(19) 0.56612(14) 0.0197(4) Uani 1 1 d . . .
H8 H 1.097933 0.234289 0.606629 0.024 Uiso 1 1 calc R U .
C9 C 1.02787(13) 0.20120(19) 0.47068(14) 0.0181(4) Uani 1 1 d . . .
H9 H 1.073908 0.237635 0.444465 0.022 Uiso 1 1 calc R U .
C10 C 0.70590(13) -0.00062(19) 0.38936(13) 0.0171(4) Uani 1 1 d . . .
C11 C 0.62730(13) 0.08047(19) 0.36336(13) 0.0179(4) Uani 1 1 d . . .
C12 C 0.56920(15) 0.2695(2) 0.30573(16) 0.0263(5) Uani 1 1 d . . .
H12 H 0.579399 0.347620 0.283071 0.032 Uiso 1 1 calc R U .
C13 C 0.47589(15) 0.2391(2) 0.30920(17) 0.0302(5) Uani 1 1 d . . .
H13 H 0.424756 0.295587 0.288269 0.036 Uiso 1 1 calc R U .
C14 C 0.45925(15) 0.1286(2) 0.34264(15) 0.0280(5) Uani 1 1 d . . .
H14 H 0.396932 0.108121 0.346764 0.034 Uiso 1 1 calc R U .
C15 C 0.53583(14) 0.0446(2) 0.37120(14) 0.0223(4) Uani 1 1 d . . .
C16 C 0.52728(15) -0.0715(2) 0.40845(15) 0.0257(5) Uani 1 1 d . . .
H16 H 0.466739 -0.097331 0.414317 0.031 Uiso 1 1 calc R U .
C17 C 0.60439(16) -0.1469(2) 0.43604(15) 0.0262(5) Uani 1 1 d . . .
H17 H 0.597412 -0.224009 0.462131 0.031 Uiso 1 1 calc R U .
C18 C 0.69486(15) -0.11171(19) 0.42628(14) 0.0211(4) Uani 1 1 d . . .
H18 H 0.748131 -0.165365 0.445430 0.025 Uiso 1 1 calc R U .
C19 C 0.8548(2) 0.4349(3) 0.53816(17) 0.0410(7) Uani 1 1 d . . .
H19A H 0.910491 0.457305 0.516579 0.061 Uiso 1 1 calc R U .
H19B H 0.869361 0.360787 0.576366 0.061 Uiso 1 1 calc R U .
H19C H 0.840150 0.500724 0.576566 0.061 Uiso 1 1 calc R U .
C20 C 0.7416(2) 0.5576(2) 0.38558(17) 0.0355(6) Uani 1 1 d . . .
H20A H 0.726212 0.616082 0.429274 0.053 Uiso 1 1 calc R U .
H20B H 0.690016 0.557452 0.325750 0.053 Uiso 1 1 calc R U .
H20C H 0.802336 0.580448 0.373524 0.053 Uiso 1 1 calc R U .
C21 C 0.73387(14) 0.2938(2) 0.20410(15) 0.0208(4) Uani 1 1 d . . .
C22 C 0.88803(14) 0.38053(19) 0.32437(14) 0.0204(4) Uani 1 1 d . . .
S1 S 0.75282(4) 0.40872(5) 0.43728(4) 0.02170(11) Uani 1 1 d . . .
O1 O 0.70133(11) 0.31199(17) 0.12382(10) 0.0303(4) Uani 1 1 d . . .
O2 O 0.93795(11) 0.45720(15) 0.31752(12) 0.0303(4) Uani 1 1 d . . .
B1 B 0.78976(18) 0.7433(2) 0.17590(17) 0.0249(5) Uani 1 1 d . . .
F1 F 0.77023(11) 0.62224(13) 0.15407(10) 0.0377(3) Uani 1 1 d . . .
F2 F 0.88762(11) 0.7636(2) 0.20322(13) 0.0717(7) Uani 1 1 d . . .
F3 F 0.74777(15) 0.81371(16) 0.09754(11) 0.0601(5) Uani 1 1 d . . .
F4 F 0.75283(9) 0.77578(12) 0.24956(9) 0.0279(3) Uani 1 1 d . . .
C1S C 0.4441(6) -0.5006(10) 0.4701(7) 0.090(3) Uani 0.5 1 d . . P
H1S1 H 0.399748 -0.568906 0.445573 0.109 Uiso 0.5 1 d R U P
H1S2 H 0.406960 -0.436418 0.491000 0.109 Uiso 0.5 1 d R U P
Cl1 Cl 0.48164(14) -0.44637(15) 0.38140(15) 0.0523(4) Uani 0.5 1 d . . P
Cl2 Cl 0.5342(2) -0.5525(3) 0.5705(2) 0.0886(8) Uani 0.5 1 d . . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C21 Mo1 C22 82.04(8) . .
C21 Mo1 N1 83.89(7) . .
C22 Mo1 N1 148.65(7) . .
C21 Mo1 C3 98.44(8) . .
C22 Mo1 C3 83.34(8) . .
N1 Mo1 C3 126.51(7) . .
C21 Mo1 C2 91.99(8) . .
C22 Mo1 C2 117.77(7) . .
N1 Mo1 C2 90.54(7) . .
C3 Mo1 C2 36.17(7) . .
C21 Mo1 C1 119.60(8) . .
C22 Mo1 C1 138.60(7) . .
N1 Mo1 C1 72.39(6) . .
C3 Mo1 C1 60.12(7) . .
C2 Mo1 C1 36.16(7) . .
C21 Mo1 C4 132.72(7) . .
C22 Mo1 C4 80.72(7) . .
N1 Mo1 C4 128.34(6) . .
C3 Mo1 C4 36.01(6) . .
C2 Mo1 C4 59.20(7) . .
C1 Mo1 C4 58.45(6) . .
C21 Mo1 C5 150.64(8) . .
C22 Mo1 C5 110.69(7) . .
N1 Mo1 C5 95.05(6) . .
C3 Mo1 C5 58.86(6) . .
C2 Mo1 C5 58.66(7) . .
C1 Mo1 C5 34.83(6) . .
C4 Mo1 C5 34.23(6) . .
C21 Mo1 S1 107.12(6) . .
C22 Mo1 S1 79.33(6) . .
N1 Mo1 S1 78.27(5) . .
C3 Mo1 S1 146.56(5) . .
C2 Mo1 S1 156.44(5) . .
C1 Mo1 S1 120.30(5) . .
C4 Mo1 S1 112.33(5) . .
C5 Mo1 S1 101.32(5) . .
C12 N1 C11 117.72(18) . .
C12 N1 Mo1 122.88(15) . .
C11 N1 Mo1 119.36(12) . .
C2 C1 C5 108.45(16) . .
C2 C1 C10 126.83(17) . .
C5 C1 C10 124.51(17) . .
C2 C1 Mo1 70.52(11) . .
C5 C1 Mo1 77.39(11) . .
C10 C1 Mo1 114.08(13) . .
C3 C2 C1 108.00(17) . .
C3 C2 Mo1 71.38(11) . .
C1 C2 Mo1 73.32(11) . .
C3 C2 H2 126.0 . .
C1 C2 H2 126.0 . .
Mo1 C2 H2 121.0 . .
C2 C3 C4 108.10(16) . .
C2 C3 Mo1 72.46(11) . .
C4 C3 Mo1 77.11(10) . .
C2 C3 H3 125.9 . .
C4 C3 H3 125.9 . .
Mo1 C3 H3 116.5 . .
C9 C4 C5 119.53(17) . .
C9 C4 C3 132.87(17) . .
C5 C4 C3 107.54(16) . .
C9 C4 Mo1 126.40(14) . .
C5 C4 Mo1 74.45(10) . .
C3 C4 Mo1 66.88(10) . .
C6 C5 C4 121.01(17) . .
C6 C5 C1 131.25(17) . .
C4 C5 C1 107.64(16) . .
C6 C5 Mo1 129.00(13) . .
C4 C5 Mo1 71.33(10) . .
C1 C5 Mo1 67.77(10) . .
C7 C6 C5 117.71(17) . .
C7 C6 H6 121.1 . .
C5 C6 H6 121.1 . .
C6 C7 C8 121.62(18) . .
C6 C7 H7 119.2 . .
C8 C7 H7 119.2 . .
C9 C8 C7 122.08(18) . .
C9 C8 H8 119.0 . .
C7 C8 H8 119.0 . .
C8 C9 C4 118.00(18) . .
C8 C9 H9 121.0 . .
C4 C9 H9 121.0 . .
C18 C10 C11 119.86(18) . .
C18 C10 C1 124.07(18) . .
C11 C10 C1 116.02(18) . .
N1 C11 C10 117.71(17) . .
N1 C11 C15 122.15(19) . .
C10 C11 C15 120.13(19) . .
N1 C12 C13 123.2(2) . .
N1 C12 H12 118.4 . .
C13 C12 H12 118.4 . .
C14 C13 C12 119.8(2) . .
C14 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
C13 C14 C15 119.25(19) . .
C13 C14 H14 120.4 . .
C15 C14 H14 120.4 . .
C16 C15 C14 124.12(19) . .
C16 C15 C11 118.11(19) . .
C14 C15 C11 117.8(2) . .
C17 C16 C15 121.00(19) . .
C17 C16 H16 119.5 . .
C15 C16 H16 119.5 . .
C16 C17 C18 120.7(2) . .
C16 C17 H17 119.7 . .
C18 C17 H17 119.7 . .
C10 C18 C17 120.2(2) . .
C10 C18 H18 119.9 . .
C17 C18 H18 119.9 . .
S1 C19 H19A 109.5 . .
S1 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
S1 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
S1 C20 H20A 109.5 . .
S1 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
S1 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
O1 C21 Mo1 173.92(19) . .
O2 C22 Mo1 177.69(19) . .
C19 S1 C20 99.09(13) . .
C19 S1 Mo1 109.28(8) . .
C20 S1 Mo1 113.50(8) . .
F2 B1 F3 109.0(2) . .
F2 B1 F1 110.5(2) . .
F3 B1 F1 109.64(19) . .
F2 B1 F4 108.92(18) . .
F3 B1 F4 109.4(2) . .
F1 B1 F4 109.39(19) . .
Cl2 C1S C1S 83.0(7) 3_646 3_646
Cl2 C1S Cl1 17.3(4) 3_646 .
C1S C1S Cl1 85.6(6) 3_646 .
Cl2 C1S Cl2 115.3(7) 3_646 .
C1S C1S Cl2 32.3(5) 3_646 .
Cl1 C1S Cl2 116.4(5) . .
Cl2 C1S Cl1 128.7(8) 3_646 3_646
C1S C1S Cl1 48.2(6) 3_646 3_646
Cl1 C1S Cl1 133.8(5) . 3_646
Cl2 C1S Cl1 19.24(18) . 3_646
Cl2 C1S H1S1 122.4 3_646 .
C1S C1S H1S1 130.9 3_646 .
Cl1 C1S H1S1 108.1 . .
Cl2 C1S H1S1 107.9 . .
Cl1 C1S H1S1 104.0 3_646 .
Cl2 C1S H1S2 93.5 3_646 .
C1S C1S H1S2 112.1 3_646 .
Cl1 C1S H1S2 108.4 . .
Cl2 C1S H1S2 108.1 . .
Cl1 C1S H1S2 92.1 3_646 .
H1S1 C1S H1S2 107.6 . .
Cl2 Cl1 C1S 20.5(5) 3_646 .
Cl2 Cl1 C1S 46.3(3) 3_646 3_646
C1S Cl1 C1S 46.2(5) . 3_646
Cl1 Cl2 C1S 142.2(8) 3_646 3_646
Cl1 Cl2 C1S 114.4(5) 3_646 .
C1S Cl2 C1S 64.7(7) 3_646 .
Cl1 Cl2 Cl2 129.4(4) 3_646 3_646
C1S Cl2 Cl2 43.1(6) 3_646 3_646
C1S Cl2 Cl2 21.6(3) . 3_646
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C21 1.937(2) .
Mo1 C22 2.034(2) .
Mo1 N1 2.2520(16) .
Mo1 C3 2.2735(18) .
Mo1 C2 2.288(2) .
Mo1 C1 2.3245(19) .
Mo1 C4 2.4097(18) .
Mo1 C5 2.4505(18) .
Mo1 S1 2.5118(5) .
N1 C12 1.329(3) .
N1 C11 1.378(3) .
C1 C2 1.432(3) .
C1 C5 1.434(3) .
C1 C10 1.475(3) .
C2 C3 1.416(3) .
C2 H2 0.9500 .
C3 C4 1.453(3) .
C3 H3 0.9500 .
C4 C9 1.425(3) .
C4 C5 1.431(3) .
C5 C6 1.419(3) .
C6 C7 1.363(3) .
C6 H6 0.9500 .
C7 C8 1.426(3) .
C7 H7 0.9500 .
C8 C9 1.363(3) .
C8 H8 0.9500 .
C9 H9 0.9500 .
C10 C18 1.368(3) .
C10 C11 1.413(3) .
C11 C15 1.420(3) .
C12 C13 1.409(3) .
C12 H12 0.9500 .
C13 C14 1.361(3) .
C13 H13 0.9500 .
C14 C15 1.415(3) .
C14 H14 0.9500 .
C15 C16 1.412(3) .
C16 C17 1.360(3) .
C16 H16 0.9500 .
C17 C18 1.414(3) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 S1 1.796(3) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 S1 1.797(2) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 O1 1.159(3) .
C22 O2 1.136(3) .
B1 F2 1.379(3) .
B1 F3 1.380(3) .
B1 F1 1.383(3) .
B1 F4 1.386(3) .
C1S Cl2 0.951(9) 3_646
C1S C1S 1.610(18) 3_646
C1S Cl1 1.662(9) .
C1S Cl2 1.766(10) .
C1S Cl1 2.223(11) 3_646
C1S H1S1 0.9900 .
C1S H1S2 0.9900 .
Cl1 Cl2 0.805(3) 3_646
Cl2 Cl2 2.336(5) 3_646
