Inorganic anion-dependent assembly of zero-, one-, two- and three-dimensional Cu(II)/Ag(I) complexes under the guidance of the HSAB theory: Synthesis, structure, and magnetic property
Liu, Yaru; Xing, Zhiyan; Zhang, Xiao; Liang, Guorui; Journal of Solid State Chemistry 246 (2017) 48–56; doi:10.1016/j.jssc.2016.10.030

data_1560636
_publ_section_title
;
 Inorganic anion-dependent assembly of zero-, one-, two- and
 three-dimensional Cu(II)/Ag(I) complexes under the guidance of the HSAB
 theory: Synthesis, structure, and magnetic property
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              48
_journal_page_last               56
_journal_paper_doi               10.1016/j.jssc.2016.10.030
_journal_volume                  246
_journal_year                    2017
_chemical_formula_moiety         'C33 H37 Cu3 N15 O S4'
_chemical_formula_sum            'C33 H37 Cu3 N15 O S4'
_chemical_formula_weight         978.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 121.531(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.5345(14)
_cell_length_b                   9.4368(4)
_cell_length_c                   18.1503(7)
_cell_measurement_reflns_used    2644
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9930
_cell_measurement_theta_min      4.9090
_cell_volume                     4165.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9737
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0332890000
_diffrn_orient_matrix_UB_12      0.0342049000
_diffrn_orient_matrix_UB_13      -0.0530968000
_diffrn_orient_matrix_UB_21      -0.0670353000
_diffrn_orient_matrix_UB_22      -0.0714999000
_diffrn_orient_matrix_UB_23      -0.0342758000
_diffrn_orient_matrix_UB_31      -0.0415851000
_diffrn_orient_matrix_UB_32      0.1426863000
_diffrn_orient_matrix_UB_33      -0.0044262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7765
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.780
_diffrn_reflns_theta_min         4.916
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1996
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.24(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         5528
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0277P)^2^+1.1819P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                4793
_reflns_number_total             5528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5.cif
_cod_data_source_block           1122-13
_cod_database_code               1560636
_chemical_oxdiff_formula         'C H N O S Cu'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C20(H20A,H20B), C24(H24A,H24B),
 C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C33(H33)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              99233
_shelx_hkl_checksum              39143