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#$Date: 2022-06-29 12:05:30 +0300 (Wed, 29 Jun 2022) $
#$Revision: 276384 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/55/8105558.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_8105558
loop_
_publ_author_name
'Zhou, Ya-Dong'
'Zheng, Yan-Rui'
'Ma, Jie'
'Deng, Yu-Heng'
_publ_section_title
;
 Crystal structure of bis(perchlorato-κ1
 O)-bis(3,4,5-trimethoxy-N-(pyridin-2-yl)benzamide-κ2 N,O)copper(II),
 C32H30Cl2CuN4O16
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              109
_journal_page_last               111
_journal_paper_doi               10.1515/ncrs-2018-0213
_journal_volume                  234
_journal_year                    2018
_chemical_formula_moiety         'C30 H32 Cu1 N4 O8, Cl2 O8'
_chemical_formula_sum            'C30 H32 Cl2 Cu N4 O16'
_chemical_formula_weight         839.05
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-07-22
_cell_angle_alpha                108.509(4)
_cell_angle_beta                 109.572(4)
_cell_angle_gamma                97.511(4)
_cell_formula_units_Z            1
_cell_length_a                   9.3135(5)
_cell_length_b                   9.5191(7)
_cell_length_c                   11.5417(6)
_cell_measurement_reflns_used    1238
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.6
_cell_measurement_theta_min      2.45
_cell_volume                     881.48(10)
_computing_cell_refinement       'Bruker SMART(Bruker 2009)'
_computing_data_collection       'Bruker SMART(Bruker 2009)'
_computing_data_reduction        'Bruker SAINT(Bruker 2009)'
_computing_molecular_graphics    'Diamond 3.2i (Brandenburg 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.950
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8594
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.031
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_correction_T_min  0.7844
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             431
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0636
_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)+(0.0854P)²+0.2331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2017
_reflns_number_total             3427
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0213_suppl.cif
_cod_data_source_block           a
_cod_original_formula_sum        'C30 H32 Cl2 Cu1 N4 O16'
_cod_database_code               8105558
_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   0.848
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O6')=Sof(O8')=Sof(O7')=1-FVAR(1)
 Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C5(H5), C12(H12), C8(H8), C2(H2A), C4(H4), C3(H3)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
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
Cu1 Cu 1.0000 0.5000 1.0000 0.0548(3) Uani 1 2 d S T P . .
Cl1 Cl 1.20239(15) 0.25711(18) 0.83616(14) 0.0699(4) Uani 1 1 d . . . . .
O1 O 1.1489(3) 0.4718(4) 1.1479(3) 0.0632(9) Uani 1 1 d . . . . .
N1 N 1.1547(4) 0.6949(5) 1.0459(4) 0.0559(10) Uani 1 1 d . . . . .
N2 N 1.3714(4) 0.6268(5) 1.1718(4) 0.0591(11) Uani 1 1 d . . . . .
H2 H 1.4718 0.6400 1.1964 0.071 Uiso 1 1 calc R . . . .
O4 O 1.3371(5) 0.2078(5) 1.4634(5) 0.0922(13) Uani 1 1 d . . . . .
C6 C 1.2968(5) 0.5121(6) 1.1908(5) 0.0575(13) Uani 1 1 d . . . . .
O2 O 1.7834(5) 0.3702(7) 1.3902(6) 0.122(2) Uani 1 1 d . . . . .
C7 C 1.3895(5) 0.4315(6) 1.2660(5) 0.0550(12) Uani 1 1 d . . . . .
C1 C 1.3097(5) 0.7283(6) 1.1179(5) 0.0550(12) Uani 1 1 d . . . . .
C5 C 1.1030(6) 0.8032(7) 1.0022(6) 0.0706(15) Uani 1 1 d . . . . .
H5 H 0.9948 0.7846 0.9557 0.085 Uiso 1 1 calc R . . . .
C12 C 1.3151(6) 0.3524(6) 1.3226(5) 0.0628(13) Uani 1 1 d . . . . .
H12 H 1.2093 0.3461 1.3067 0.075 Uiso 1 1 calc R . . . .
C11 C 1.3977(7) 0.2840(7) 1.4016(6) 0.0706(15) Uani 1 1 d . . . . .
C8 C 1.5440(5) 0.4366(7) 1.2850(5) 0.0643(14) Uani 1 1 d . . . . .
H8 H 1.5924 0.4863 1.2449 0.077 Uiso 1 1 calc R . . . .
C2 C 1.4127(6) 0.8625(7) 1.1411(6) 0.0752(16) Uani 1 1 d . . . . .
H2A H 1.5205 0.8812 1.1893 0.090 Uiso 1 1 calc R . . . .
C4 C 1.1970(7) 0.9348(7) 1.0215(6) 0.0811(17) Uani 1 1 d . . . . .
H4 H 1.1545 1.0027 0.9864 0.097 Uiso 1 1 calc R . . . .
O3 O 1.6387(7) 0.2431(9) 1.5183(6) 0.155(3) Uani 1 1 d . . . . .
C3 C 1.3560(7) 0.9685(7) 1.0932(7) 0.0837(18) Uani 1 1 d . . . . .
H3 H 1.4237 1.0598 1.1092 0.100 Uiso 1 1 calc R . . . .
C9 C 1.6275(6) 0.3670(8) 1.3644(6) 0.0785(17) Uani 1 1 d . . . . .
C10 C 1.5555(7) 0.2915(8) 1.4250(6) 0.0836(19) Uani 1 1 d . . . . .
C15 C 1.1734(8) 0.1830(9) 1.4315(8) 0.106(2) Uani 1 1 d . . . . .
H15A H 1.1437 0.1251 1.4782 0.159 Uiso 1 1 calc GR . . . .
H15B H 1.1162 0.1270 1.3371 0.159 Uiso 1 1 calc GR . . . .
H15C H 1.1489 0.2802 1.4573 0.159 Uiso 1 1 calc GR . . . .
C13 C 1.8502(9) 0.4161(13) 1.3111(9) 0.151(4) Uani 1 1 d . . . . .
H13A H 1.9521 0.3961 1.3285 0.227 Uiso 1 1 calc GR . . . .
H13B H 1.8615 0.5240 1.3321 0.227 Uiso 1 1 calc GR . . . .
H13C H 1.7826 0.3596 1.2186 0.227 Uiso 1 1 calc GR . . . .
C14 C 1.7232(14) 0.1561(14) 1.5146(11) 0.192(5) Uani 1 1 d . . . . .
H14A H 1.7588 0.1414 1.5971 0.288 Uiso 1 1 calc GR . . . .
H14B H 1.8127 0.1991 1.5015 0.288 Uiso 1 1 calc GR . . . .
H14C H 1.6646 0.0590 1.4423 0.288 Uiso 1 1 calc GR . . . .
O6 O 1.2795(7) 0.2644(9) 0.7532(7) 0.099(3) Uani 0.762(10) 1 d . . . . .
O7 O 1.3035(11) 0.2576(11) 0.9603(6) 0.123(3) Uani 0.762(10) 1 d . . . . .
O8 O 1.0876(13) 0.1169(11) 0.7763(12) 0.213(6) Uani 0.762(10) 1 d . . . . .
O6' O 1.339(2) 0.384(2) 0.889(2) 0.095(7) Uiso 0.238(10) 1 d . . . . .
O8' O 1.179(3) 0.164(3) 0.714(2) 0.118(9) Uiso 0.238(10) 1 d . . . . .
O7' O 1.218(3) 0.173(4) 0.903(3) 0.112(9) Uiso 0.238(10) 1 d . . . . .
O5 O 1.1130(7) 0.3622(8) 0.8495(6) 0.144(2) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O1 Cu1 O1 180.0(2) 2_767 .
O1 Cu1 N1 91.32(15) 2_767 .
O1 Cu1 N1 88.68(15) . .
O1 Cu1 N1 91.32(15) . 2_767
O1 Cu1 N1 88.68(15) 2_767 2_767
N1 Cu1 N1 180.0 2_767 .
O6 Cl1 O7 113.1(4) . .
O6 Cl1 O8 109.0(6) . .
O8 Cl1 O7 104.5(6) . .
O8' Cl1 O6' 110.6(15) . .
O8' Cl1 O5 118.6(11) . .
O7' Cl1 O6' 112.3(16) . .
O7' Cl1 O8' 104.6(18) . .
O7' Cl1 O5 121.4(12) . .
O5 Cl1 O6 113.5(3) . .
O5 Cl1 O7 113.4(4) . .
O5 Cl1 O8 102.2(6) . .
O5 Cl1 O6' 88.4(9) . .
C6 O1 Cu1 126.8(3) . .
C1 N1 Cu1 124.3(3) . .
C1 N1 C5 116.3(5) . .
C5 N1 Cu1 119.4(3) . .
C6 N2 C1 129.2(4) . .
C11 O4 C15 117.0(5) . .
O1 C6 N2 121.6(4) . .
O1 C6 C7 118.7(5) . .
N2 C6 C7 119.7(4) . .
C9 O2 C13 118.0(5) . .
C12 C7 C6 117.1(4) . .
C8 C7 C6 122.6(5) . .
C8 C7 C12 120.3(4) . .
N1 C1 N2 120.0(4) . .
N1 C1 C2 121.8(5) . .
C2 C1 N2 118.3(4) . .
C4 C5 N1 124.5(5) . .
C11 C12 C7 120.2(5) . .
O4 C11 C12 124.6(5) . .
O4 C11 C10 115.0(5) . .
C12 C11 C10 120.4(5) . .
C7 C8 C9 119.6(5) . .
C3 C2 C1 120.2(5) . .
C5 C4 C3 119.5(5) . .
C14 O3 C10 131.2(8) . .
C4 C3 C2 117.7(6) . .
O2 C9 C8 122.9(5) . .
O2 C9 C10 116.5(5) . .
C8 C9 C10 120.6(5) . .
C11 C10 C9 118.9(5) . .
O3 C10 C11 118.4(6) . .
O3 C10 C9 122.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.926(3) 2_767
Cu1 O1 1.926(3) .
Cu1 N1 1.991(4) .
Cu1 N1 1.991(4) 2_767
Cl1 O6 1.388(5) .
Cl1 O7 1.425(6) .
Cl1 O8 1.396(8) .
Cl1 O5 1.387(5) .
O1 C6 1.255(5) .
N1 C1 1.335(6) .
N1 C5 1.358(6) .
N2 C6 1.334(6) .
N2 C1 1.393(6) .
O4 C11 1.358(6) .
O4 C15 1.411(7) .
C6 C7 1.477(6) .
O2 C9 1.375(6) .
O2 C13 1.405(7) .
C7 C12 1.397(7) .
C7 C8 1.373(6) .
C1 C2 1.383(7) .
C5 C4 1.338(7) .
C12 C11 1.373(7) .
C11 C10 1.390(7) .
C8 C9 1.387(7) .
C2 C3 1.379(8) .
C4 C3 1.366(8) .
O3 C10 1.349(6) .
O3 C14 1.215(9) .
C9 C10 1.402(8) .
