Crystal structure of bis(perchlorato-κ1 O)-bis(3,4,5-trimethoxy-N-(pyridin-2-yl)benzamide-κ2 N,O)copper(II), C32H30Cl2CuN4O16
Zhou, Ya-Dong; Zheng, Yan-Rui; Ma, Jie; Deng, Yu-Heng; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 109–111; doi:10.1515/ncrs-2018-0213

data_8105558
_publ_section_title
;
 Crystal structure of bis(perchlorato-\k1
 O)-bis(3,4,5-trimethoxy-N-(pyridin-2-yl)benzamide-\k2 N,O)copper(II),
 C32H30Cl2CuN4O16
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur 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       '\f and \w 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/[\s^2^(Fo^2^)+(0.0854P)^2^+0.2331P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;