#------------------------------------------------------------------------------
#$Date: 2019-11-05 20:18:30 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223360 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/17/7701795.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_7701795
loop_
_publ_author_name
'Hu, Min-Na'
'Zhang, Wen-Qian'
'Liu, Hua'
'He, Peng-Xiu'
'Liu, Ping'
'Wang, Yao-Yu'
'Li, Jian-Li'
_publ_section_title
;
 Five complexes based on a new racemic tetraoxaspiro ligand: correlation
 of potential coordination preferences with the structure, magnetic
 properties and luminescence properties.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3862
_journal_page_last               3873
_journal_paper_doi               10.1039/c8dt04051f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C40 H50 Cd3 Cl6 N6 O10'
_chemical_formula_weight         1324.76
_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   geom
_audit_block_doi                 10.5517/ccdc.csd.cc205mrl
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-25 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                112.424(2)
_cell_angle_beta                 105.362(2)
_cell_angle_gamma                96.032(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5000(16)
_cell_length_b                   10.7183(17)
_cell_length_c                   13.594(2)
_cell_measurement_reflns_used    2417
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.03
_cell_volume                     1200.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7199
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.609
_diffrn_reflns_theta_min         2.078
_exptl_absorpt_coefficient_mu    1.711
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       block
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.501
_refine_diff_density_min         -2.745
_refine_diff_density_rms         0.523
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0535
_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)+(0.1892P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.2545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3990
_reflns_number_total             5276
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04051f2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1200.3(3)
_cod_database_code               7701795
_shelx_shelxl_version_number     2014/7
_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   0.771
_shelx_estimated_absorpt_t_max   0.834
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
C1 C 0.9293(9) 0.9208(8) 0.6290(7) 0.0332(18) Uani 1 1 d . . .
H1 H 0.8570 0.9502 0.5875 0.040 Uiso 1 1 calc R U .
C2 C 1.0806(10) 0.9875(9) 0.6656(9) 0.043(2) Uani 1 1 d . . .
H2 H 1.1091 1.0591 0.6471 0.052 Uiso 1 1 calc R U .
C3 C 1.1876(9) 0.9454(9) 0.7298(7) 0.0331(17) Uani 1 1 d . . .
H3 H 1.2886 0.9883 0.7538 0.040 Uiso 1 1 calc R U .
C4 C 1.1453(8) 0.8415(8) 0.7577(6) 0.0281(16) Uani 1 1 d . . .
C5 C 0.9945(9) 0.7762(8) 0.7144(6) 0.0275(16) Uani 1 1 d . . .
H5 H 0.9665 0.7009 0.7289 0.033 Uiso 1 1 calc R U .
C6 C 1.2573(8) 0.7997(7) 0.8294(6) 0.0242(14) Uani 1 1 d . . .
H6 H 1.3496 0.8049 0.8104 0.029 Uiso 1 1 calc R U .
C7 C 1.3988(9) 0.8749(8) 1.0198(6) 0.0281(16) Uani 1 1 d . . .
H7A H 1.4141 0.9433 1.0955 0.034 Uiso 1 1 calc R U .
H7B H 1.4926 0.8851 1.0048 0.034 Uiso 1 1 calc R U .
C8 C 1.3543(8) 0.7290(7) 1.0125(6) 0.0245(15) Uani 1 1 d . . .
C9 C 1.3159(8) 0.6288(7) 0.8900(6) 0.0261(15) Uani 1 1 d . . .
H9A H 1.4062 0.6281 0.8695 0.031 Uiso 1 1 calc R U .
H9B H 1.2760 0.5359 0.8797 0.031 Uiso 1 1 calc R U .
C10 C 1.4835(8) 0.7011(7) 1.0902(6) 0.0260(15) Uani 1 1 d . . .
H10A H 1.5680 0.6978 1.0626 0.031 Uiso 1 1 calc R U .
H10B H 1.5157 0.7758 1.1655 0.031 Uiso 1 1 calc R U .
C11 C 1.2246(9) 0.7213(9) 1.0542(7) 0.0332(18) Uani 1 1 d . . .
H11A H 1.2496 0.7949 1.1294 0.040 Uiso 1 1 calc R U .
H11B H 1.1383 0.7341 1.0050 0.040 Uiso 1 1 calc R U .
C12 C 1.3066(9) 0.5724(9) 1.1312(7) 0.0315(17) Uani 1 1 d . . .
H12 H 1.3308 0.6476 1.2067 0.038 Uiso 1 1 calc R U .
C13 C 1.2757(8) 0.4380(8) 1.1353(6) 0.0270(16) Uani 1 1 d . . .
C14 C 1.1967(10) 0.3193(9) 1.0406(7) 0.0361(19) Uani 1 1 d . . .
H14 H 1.1548 0.3241 0.9724 0.043 Uiso 1 1 calc R U .
C15 C 1.1788(10) 0.1920(9) 1.0454(7) 0.0365(19) Uani 1 1 d . . .
H15 H 1.1243 0.1114 0.9814 0.044 Uiso 1 1 calc R U .
C16 C 1.2442(9) 0.1873(8) 1.1484(7) 0.0301(17) Uani 1 1 d . . .
H16 H 1.2371 0.1018 1.1516 0.036 Uiso 1 1 calc R U .
C17 C 1.3315(9) 0.4232(8) 1.2348(7) 0.0311(17) Uani 1 1 d . . .
H17 H 1.3827 0.5033 1.3003 0.037 Uiso 1 1 calc R U .
C18 C 0.1932(9) 0.7858(8) 0.4389(7) 0.0307(17) Uani 1 1 d . . .
H18 H 0.2318 0.7968 0.5129 0.037 Uiso 1 1 calc R U .
C19 C -0.0219(14) 0.6218(10) 0.4155(8) 0.058(3) Uani 1 1 d . . .
H19A H 0.0428 0.6215 0.4829 0.087 Uiso 1 1 calc R U .
H19B H -0.0651 0.5280 0.3595 0.087 Uiso 1 1 calc R U .
H19C H -0.1004 0.6667 0.4322 0.087 Uiso 1 1 calc R U .
C20 C -0.0007(14) 0.6714(12) 0.2548(9) 0.063(3) Uani 1 1 d . . .
H20A H 0.0277 0.7542 0.2462 0.094 Uiso 1 1 calc R U .
H20B H -0.1080 0.6451 0.2326 0.094 Uiso 1 1 calc R U .
H20C H 0.0347 0.5980 0.2082 0.094 Uiso 1 1 calc R U .
Cd1 Cd 0.61623(6) 0.69889(5) 0.57678(4) 0.0244(2) Uani 1 1 d . . .
Cd2 Cd 0.5000 1.0000 0.5000 0.0244(2) Uani 1 2 d S . P
Cl1 Cl 0.5368(2) 0.9340(2) 0.66978(16) 0.0293(4) Uani 1 1 d . . .
Cl2 Cl 0.6003(2) 0.7744(2) 0.41250(16) 0.0296(4) Uani 1 1 d . . .
Cl3 Cl 0.6600(2) 0.4527(2) 0.4768(2) 0.0352(5) Uani 1 1 d . . .
N1 N 0.8856(7) 0.8131(7) 0.6531(6) 0.0278(14) Uani 1 1 d . . .
N2 N 1.3174(8) 0.3039(7) 1.2434(5) 0.0282(14) Uani 1 1 d . . .
N3 N 0.0652(7) 0.6969(7) 0.3724(6) 0.0326(15) Uani 1 1 d . . .
O1 O 1.2095(6) 0.6670(5) 0.8194(5) 0.0316(12) Uani 1 1 d . . .
O2 O 1.2860(6) 0.8995(5) 0.9407(4) 0.0287(12) Uani 1 1 d . . .
O3 O 1.1883(6) 0.5883(6) 1.0566(5) 0.0318(12) Uani 1 1 d . . .
O4 O 1.4372(5) 0.5731(6) 1.0942(5) 0.0271(11) Uani 1 1 d . . .
O5 O 0.2652(6) 0.8569(6) 0.4043(5) 0.0370(14) Uani 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
N1 C1 C2 121.3(7) . .
C3 C2 C1 119.1(8) . .
C4 C3 C2 120.3(8) . .
C3 C4 C5 117.4(7) . .
C3 C4 C6 120.6(7) . .
C5 C4 C6 122.0(7) . .
N1 C5 C4 125.1(7) . .
O1 C6 O2 110.6(6) . .
O1 C6 C4 113.6(6) . .
O2 C6 C4 105.1(6) . .
O2 C7 C8 111.4(6) . .
C11 C8 C9 112.3(6) . .
C11 C8 C10 106.8(6) . .
C9 C8 C10 112.1(6) . .
C11 C8 C7 109.2(6) . .
C9 C8 C7 106.5(6) . .
C10 C8 C7 110.0(6) . .
O1 C9 C8 110.8(6) . .
O4 C10 C8 110.3(6) . .
O3 C11 C8 110.2(6) . .
O3 C12 O4 110.0(6) . .
O3 C12 C13 112.2(7) . .
O4 C12 C13 104.9(6) . .
C14 C13 C17 116.5(7) . .
C14 C13 C12 121.8(7) . .
C17 C13 C12 121.6(7) . .
C13 C14 C15 120.6(7) . .
C14 C15 C16 118.6(7) . .
N2 C16 C15 121.6(7) . .
N2 C17 C13 125.0(7) . .
O5 C18 N3 121.3(8) . .
N2 Cd1 N1 79.4(2) 2_767 .
N2 Cd1 Cl3 93.72(17) 2_767 .
N1 Cd1 Cl3 93.87(16) . .
N2 Cd1 Cl2 162.78(17) 2_767 .
N1 Cd1 Cl2 86.78(16) . .
Cl3 Cd1 Cl2 97.39(7) . .
N2 Cd1 Cl1 87.16(17) 2_767 .
N1 Cd1 Cl1 93.11(16) . .
Cl3 Cd1 Cl1 173.01(7) . .
Cl2 Cd1 Cl1 83.42(6) . .
N2 Cd1 Cl3 89.63(17) 2_767 2_666
N1 Cd1 Cl3 167.59(16) . 2_666
Cl3 Cd1 Cl3 81.05(7) . 2_666
Cl2 Cd1 Cl3 105.04(7) . 2_666
Cl1 Cd1 Cl3 92.03(6) . 2_666
O5 Cd2 O5 180.0 2_676 .
O5 Cd2 Cl1 93.08(16) 2_676 2_676
O5 Cd2 Cl1 86.92(16) . 2_676
O5 Cd2 Cl1 86.92(16) 2_676 .
O5 Cd2 Cl1 93.08(16) . .
Cl1 Cd2 Cl1 180.00(7) 2_676 .
O5 Cd2 Cl2 85.78(17) 2_676 2_676
O5 Cd2 Cl2 94.22(17) . 2_676
Cl1 Cd2 Cl2 83.44(6) 2_676 2_676
Cl1 Cd2 Cl2 96.56(6) . 2_676
O5 Cd2 Cl2 94.22(17) 2_676 .
O5 Cd2 Cl2 85.78(17) . .
Cl1 Cd2 Cl2 96.56(6) 2_676 .
Cl1 Cd2 Cl2 83.44(6) . .
Cl2 Cd2 Cl2 180.00(11) 2_676 .
Cd2 Cl1 Cd1 96.73(6) . .
Cd1 Cl2 Cd2 96.11(6) . .
Cd1 Cl3 Cd1 98.95(7) . 2_666
C5 N1 C1 116.8(7) . .
C5 N1 Cd1 125.4(5) . .
C1 N1 Cd1 117.8(5) . .
C17 N2 C16 117.7(6) . .
C17 N2 Cd1 120.3(5) . 2_767
C16 N2 Cd1 121.2(5) . 2_767
C18 N3 C20 122.6(8) . .
C18 N3 C19 120.7(8) . .
C20 N3 C19 116.6(8) . .
C6 O1 C9 113.3(5) . .
C6 O2 C7 111.2(6) . .
C12 O3 C11 110.2(6) . .
C10 O4 C12 111.0(6) . .
C18 O5 Cd2 126.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.368(10) .
C1 C2 1.400(11) .
C2 C3 1.388(11) .
C3 C4 1.362(11) .
C4 C5 1.384(11) .
C4 C6 1.472(10) .
C5 N1 1.342(10) .
C6 O1 1.391(8) .
C6 O2 1.411(9) .
C7 O2 1.428(9) .
C7 C8 1.535(10) .
C8 C11 1.493(11) .
C8 C9 1.513(10) .
C8 C10 1.531(10) .
C9 O1 1.408(8) .
C10 O4 1.422(9) .
C11 O3 1.446(9) .
C12 O3 1.374(9) .
C12 O4 1.457(9) .
C12 C13 1.465(11) .
C13 C14 1.371(11) .
C13 C17 1.392(11) .
C14 C15 1.386(12) .
C15 C16 1.395(11) .
C16 N2 1.351(10) .
C17 N2 1.324(10) .
C18 O5 1.266(10) .
C18 N3 1.311(10) .
C19 N3 1.467(11) .
C20 N3 1.456(12) .
Cd1 N2 2.370(6) 2_767
Cd1 N1 2.468(6) .
Cd1 Cl3 2.603(2) .
Cd1 Cl2 2.625(2) .
Cd1 Cl1 2.645(2) .
Cd1 Cl3 2.692(2) 2_666
Cd2 O5 2.289(5) 2_676
Cd2 O5 2.289(5) .
Cd2 Cl1 2.6113(19) 2_676
Cd2 Cl1 2.6113(19) .
Cd2 Cl2 2.657(2) 2_676
Cd2 Cl2 2.657(2) .
Cl3 Cd1 2.692(2) 2_666
N2 Cd1 2.370(6) 2_767
