Anionic metal-organic framework for adsorption and separation of light hydrocarbons.
Li, Jia; Fu, Hong-Ru; Zhang, Jian; Zheng, Lan-Sun; Tao, Jun; Inorganic chemistry 54 (2015) 3093–3095; doi:10.1021/acs.inorgchem.5b00316

data_4346109
_publ_section_title
;
 Anionic metal-organic framework for adsorption and separation of light
 hydrocarbons.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3093
_journal_page_last               3095
_journal_paper_doi               10.1021/acs.inorgchem.5b00316
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '0.17(C204 H132 N24 Ni18 O84 S12)'
_chemical_formula_sum            'C34 H22 N4 Ni3 O14 S2'
_chemical_formula_weight         950.81
_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_Hall           '-I 2 2 3'
_space_group_name_H-M_alt        'I m -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-07
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   26.7674(5)
_cell_length_b                   26.7674(5)
_cell_length_c                   26.7674(5)
_cell_measurement_reflns_used    1921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.8490
_cell_measurement_theta_min      3.9670
_cell_volume                     19178.7(6)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1240
_diffrn_reflns_av_unetI/netI     0.1265
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            8128
_diffrn_reflns_theta_full        73.99
_diffrn_reflns_theta_max         73.99
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.017
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5784
_platon_squeeze_details
;
;
_refine_diff_density_max         2.384
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.321
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.321
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.1055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2637
_refine_ls_wR_factor_ref         0.2833
_reflns_number_gt                2159
_reflns_number_total             3390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00316_si_002.cif
_cod_data_source_block           p
_cod_database_code               4346109
_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. Others
 Fixed Sof: S2(0.25) H9a(0.5) H9b(0.5)
3.a Riding coordinates:
 C9(H9a,H9b,H9c)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C3(H3)
;