Crystal structure of (1,4-diazepane)4CuII 2(μ-Cl)10CuI 6, C20H48Cl10Cu8N8
Xing, Zheng; Yin, Heng-Bo; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 391–392; doi:10.1515/ncrs-2018-0185

data_8105655
_publ_section_title
;
 Crystal structure of (1,4-diazepane)4CuII 2(\m-Cl)10CuI 6,
 C20H48Cl10Cu8N8
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              391
_journal_page_last               392
_journal_paper_doi               10.1515/ncrs-2018-0185
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C20 H48 Cl10 Cu8 N8'
_chemical_formula_sum            'C20 H48 Cl10 Cu8 N8'
_chemical_formula_weight         1263.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-06
_audit_creation_method           SHELXL-2015
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.477(10)
_cell_length_b                   10.008(6)
_cell_length_c                   24.201(15)
_cell_measurement_reflns_used    2356
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.445
_cell_measurement_theta_min      2.473
_cell_volume                     3991(4)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Diamond 3.2i[4]'
_computing_publication_material  Olex2-2009[3]
_computing_structure_refinement  ShelXL-2015[2]
_computing_structure_solution    ShelXL-2015[2]
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            8599
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.462
_diffrn_reflns_theta_min         2.991
_exptl_absorpt_coefficient_mu    4.875
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0303P)^2^+8.2774P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1691
_reflns_number_total             2291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0185_suppl.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               8105655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
;