#------------------------------------------------------------------------------
#$Date: 2021-05-05 11:02:42 +0300 (Wed, 05 May 2021) $
#$Revision: 264865 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/80/7128075.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_7128075
loop_
_publ_author_name
'Voigt, Laura'
'Wugt Larsen, René'
'Kubus, Mariusz'
'Pedersen, Kasper S.'
_publ_section_title
;
 Zero-valent metals in metal-organic frameworks:
 fac-M(CO)₃(pyrazine)<sub>3/2</sub>.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3861
_journal_page_last               3864
_journal_paper_doi               10.1039/d1cc00864a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C9 H6 Mo N3 O3, C2 H2 N'
_chemical_formula_sum            'C11 H8 Mo N4 O3'
_chemical_formula_weight         340.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                64.131(10)
_cell_angle_beta                 88.185(9)
_cell_angle_gamma                86.345(10)
_cell_formula_units_Z            2
_cell_length_a                   6.8571(8)
_cell_length_b                   9.7204(11)
_cell_length_c                   10.0406(10)
_cell_measurement_reflns_used    1262
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.0670
_cell_measurement_theta_min      4.7810
_cell_volume                     600.95(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  39.00   1.00  110.00    --   10.87 -99.00 120.00   26
  2  ω    -57.00  34.00   1.00  110.00    --   10.87 -57.00 120.00   91
  3  ω    -15.00  77.00   1.00  110.00    --   10.87  77.00  30.00   92
  4  ω    -16.00  83.00   1.00  110.00    --   10.87  57.00 -90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0878018000
_diffrn_orient_matrix_UB_12      -0.0467549000
_diffrn_orient_matrix_UB_13      0.0211321000
_diffrn_orient_matrix_UB_21      0.0531043000
_diffrn_orient_matrix_UB_22      0.0655437000
_diffrn_orient_matrix_UB_23      -0.0151634000
_diffrn_orient_matrix_UB_31      -0.0146481000
_diffrn_orient_matrix_UB_32      -0.0107264000
_diffrn_orient_matrix_UB_33      0.0740777000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1047
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       needle
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0249P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3081
_reflns_number_total             4212
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -179.9834° 
 around [0.03 0.67 -0.75] (reciprocal) or [-0.00 0.71 -0.71] (direct)
;
_cod_data_source_file            d1cc00864a2.cif
_cod_data_source_block           lv194_moco3pyz2_e_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7128075--7128079.cif.'
_cod_database_code               7128075
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H16 Mo2 N8 O8'
_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_max   0.978
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6022(9)
 0.3978(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C7(H7), C9(H9), C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.672
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.33092(6) 0.65555(5) 0.17640(4) 0.00945(11) Uani 1 1 d . . . . .
N1 N 0.1204(6) 0.8639(4) 0.0709(4) 0.0100(9) Uani 1 1 d . . . . .
O1 O 0.5743(4) 0.8308(4) 0.3034(3) 0.0202(7) Uani 1 1 d . . . . .
N3 N 0.1263(6) 0.5635(4) 0.3760(4) 0.0101(9) Uani 1 1 d . . . . .
N4 N 0.1306(5) 0.5532(4) 0.0711(4) 0.0093(8) Uani 1 1 d . . . . .
O2 O 0.5941(5) 0.7658(4) -0.1065(3) 0.0213(8) Uani 1 1 d . . . . .
C1 C 0.4831(6) 0.7625(5) 0.2579(5) 0.0152(10) Uani 1 1 d . . . . .
C2 C 0.4956(8) 0.7261(5) -0.0002(5) 0.0133(12) Uani 1 1 d . . . . .
O3 O 0.6410(6) 0.3838(4) 0.3230(4) 0.0290(9) Uani 1 1 d . . . . .
C3 C 0.5194(8) 0.4825(6) 0.2677(5) 0.0149(11) Uani 1 1 d . . . . .
C4 C 0.0447(8) 0.4193(5) 0.1419(5) 0.0149(11) Uani 1 1 d . . . . .
H4 H 0.072492 0.359460 0.241496 0.018 Uiso 1 1 calc R U . . .
C5 C 0.0828(7) 0.6329(5) -0.0729(5) 0.0134(11) Uani 1 1 d . . . . .
H5 H 0.137721 0.726461 -0.127636 0.016 Uiso 1 1 calc R U . . .
C6 C -0.0723(6) 0.8627(5) 0.0551(4) 0.0115(10) Uani 1 1 d . . . . .
H6 H -0.129709 0.768875 0.092394 0.014 Uiso 1 1 calc R U . . .
C8 C 0.1381(7) 0.4132(5) 0.4731(4) 0.0128(10) Uani 1 1 d . . . . .
H8 H 0.233334 0.348516 0.458510 0.015 Uiso 1 1 calc R U . . .
C7 C 0.1903(7) 1.0046(5) 0.0146(4) 0.0108(10) Uani 1 1 d . . . . .
H7 H 0.323158 1.013192 0.022915 0.013 Uiso 1 1 calc R U . . .
C9 C -0.0126(7) 0.6473(5) 0.4066(4) 0.0134(11) Uani 1 1 d . . . . .
H9 H -0.026407 0.751567 0.344358 0.016 Uiso 1 1 calc R U . . .
N5 N 0.0208(7) 0.9805(5) -0.3547(4) 0.0265(11) Uani 1 1 d . . . . .
C10 C -0.1518(8) 1.0024(6) -0.4180(6) 0.0257(12) Uani 1 1 d . . . . .
C11 C 0.1720(7) 0.9786(5) -0.4387(5) 0.0264(12) Uani 1 1 d . . . . .
H11 H 0.296963 0.963960 -0.399714 0.032 Uiso 1 1 calc R U . . .
H10 H -0.263(8) 0.997(6) -0.357(6) 0.038(16) Uiso 1 1 d . . . . .
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'
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'
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
_geom_angle_publ_flag
N1 Mo1 N3 88.55(12) . . ?
N1 Mo1 N4 83.07(13) . . ?
N4 Mo1 N3 85.90(13) . . ?
C1 Mo1 N1 90.78(16) . . ?
C1 Mo1 N3 93.73(16) . . ?
C1 Mo1 N4 173.85(15) . . ?
C1 Mo1 C2 90.42(19) . . ?
C1 Mo1 C3 86.93(19) . . ?
C2 Mo1 N1 91.56(18) . . ?
C2 Mo1 N3 175.84(17) . . ?
C2 Mo1 N4 89.98(16) . . ?
C3 Mo1 N1 177.59(19) . . ?
C3 Mo1 N3 92.35(18) . . ?
C3 Mo1 N4 99.22(17) . . ?
C3 Mo1 C2 87.70(18) . . ?
C6 N1 Mo1 126.3(3) . . ?
C6 N1 C7 114.5(4) . . ?
C7 N1 Mo1 119.2(3) . . ?
C8 N3 Mo1 120.7(3) . . ?
C9 N3 Mo1 124.6(3) . . ?
C9 N3 C8 114.7(4) . . ?
C4 N4 Mo1 125.7(3) . . ?
C4 N4 C5 114.9(4) . . ?
C5 N4 Mo1 119.3(3) . . ?
O1 C1 Mo1 178.1(4) . . ?
O2 C2 Mo1 178.6(4) . . ?
O3 C3 Mo1 176.0(5) . . ?
N4 C4 H4 118.6 . . ?
N4 C4 C5 122.7(4) . 2_565 ?
C5 C4 H4 118.6 2_565 . ?
N4 C5 C4 122.3(4) . 2_565 ?
N4 C5 H5 118.8 . . ?
C4 C5 H5 118.8 2_565 . ?
N1 C6 H6 118.6 . . ?
N1 C6 C7 122.8(4) . 2_575 ?
C7 C6 H6 118.6 2_575 . ?
N3 C8 H8 118.9 . . ?
N3 C8 C9 122.2(4) . 2_566 ?
C9 C8 H8 118.9 2_566 . ?
N1 C7 C6 122.7(4) . 2_575 ?
N1 C7 H7 118.6 . . ?
C6 C7 H7 118.6 2_575 . ?
N3 C9 C8 123.2(4) . 2_566 ?
N3 C9 H9 118.4 . . ?
C8 C9 H9 118.4 2_566 . ?
C11 N5 C10 115.2(4) . . ?
N5 C10 C11 122.3(5) . 2_574 ?
N5 C10 H10 116(3) . . ?
C11 C10 H10 121(3) 2_574 . ?
N5 C11 C10 122.5(5) . 2_574 ?
N5 C11 H11 118.7 . . ?
C10 C11 H11 118.7 2_574 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 N1 2.271(4) . ?
Mo1 N3 2.281(4) . ?
Mo1 N4 2.276(3) . ?
Mo1 C1 1.943(5) . ?
Mo1 C2 1.949(5) . ?
Mo1 C3 1.948(5) . ?
N1 C6 1.337(6) . ?
N1 C7 1.346(6) . ?
O1 C1 1.173(5) . ?
N3 C8 1.356(5) . ?
N3 C9 1.330(6) . ?
N4 C4 1.345(6) . ?
N4 C5 1.349(5) . ?
O2 C2 1.172(6) . ?
O3 C3 1.177(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(6) 2_565 ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.387(6) 2_575 ?
C8 H8 0.9300 . ?
C8 C9 1.387(6) 2_566 ?
C7 H7 0.9300 . ?
C9 H9 0.9300 . ?
N5 C10 1.321(6) . ?
N5 C11 1.320(6) . ?
C10 C11 1.379(7) 2_574 ?
C10 H10 0.95(6) . ?
C11 H11 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 N1 C6 C7 -178.1(3) . . . 2_575 ?
Mo1 N1 C7 C6 178.2(3) . . . 2_575 ?
Mo1 N3 C8 C9 -178.3(3) . . . 2_566 ?
Mo1 N3 C9 C8 178.3(3) . . . 2_566 ?
Mo1 N4 C4 C5 176.9(3) . . . 2_565 ?
Mo1 N4 C5 C4 -177.1(3) . . . 2_565 ?
C4 N4 C5 C4 0.1(7) . . . 2_565 ?
C5 N4 C4 C5 -0.1(7) . . . 2_565 ?
C6 N1 C7 C6 -0.6(7) . . . 2_575 ?
C8 N3 C9 C8 -0.8(7) . . . 2_566 ?
C7 N1 C6 C7 0.6(7) . . . 2_575 ?
C9 N3 C8 C9 0.8(7) . . . 2_566 ?
C10 N5 C11 C10 -0.2(8) . . . 2_574 ?
C11 N5 C10 C11 0.2(8) . . . 2_574 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6022(9) 2924 2079 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.3978(9) 2942 2079 nmt -1.0004 0.0354 -0.0355 -0.0011 -0.0567 -0.9446 0.0020
-1.0575 0.0582
