An antiferromagnetic metalloring pyrazolate (Pz) framework with [Cu12(μ2-OH)12(Pz)12] nodes for separation of C2H2/CH4 mixture
Li, Ziyin; Ye, Yingxiang; Yao, Zizhu; Guo, Junzhi; Lin, Quanjie; Zhang, Jindan; Zhang, Zhangjing; Wei, Fangfang; Xiang, Shengchang; Journal of Materials Chemistry A 6 (2018) 19681–; doi:10.1039/C8TA04498H

data_7237154
_publ_section_title
;
 An antiferromagnetic metalloring pyrazolate (Pz) framework with
 [Cu12(\m2-OH)12(Pz)12] nodes for separation of C2H2/CH4 mixture
;
_journal_issue                   40
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              19681
_journal_paper_doi               10.1039/C8TA04498H
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C48 H36 Cu4 N12 O12'
_chemical_formula_sum            'C48 H36 Cu4 N12 O12'
_chemical_formula_weight         1227.05
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-04-10 deposited with the CCDC.
2018-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   26.0992(4)
_cell_length_b                   26.0992(4)
_cell_length_c                   9.2584(2)
_cell_measurement_reflns_used    3469
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.9460
_cell_measurement_theta_min      3.3380
_cell_volume                     5461.61(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_number            18435
_diffrn_reflns_point_group_measured_fraction_full 0.732
_diffrn_reflns_point_group_measured_fraction_max 0.693
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.036
_diffrn_reflns_theta_min         3.387
_exptl_absorpt_coefficient_mu    1.755
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_F_000             1860
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         10281
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0250P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.463
_reflns_Friedel_fraction_full    0.483
_reflns_Friedel_fraction_max     0.439
_reflns_number_gt                7079
_reflns_number_total             10281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta04498h2.cif
_cod_data_source_block           a_sq_s
_cod_original_cell_volume        5461.6(2)
_cod_database_code               7237154
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4
 0.8 with sigma of 0.02
 O3-H3
 0.8 with sigma of 0.02
 O2-H2
 0.8 with sigma of 0.02
 O1-H1
 0.8 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C46(H46), C37(H37), C8(H8), C41(H41), C12(H12), C13(H13), C42(H42)
3.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C),
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              78505
_shelx_fab_checksum              55921
_olex2_submission_special_instructions 'No special instructions were received'