A spin-canted NiII4-based metal-organic framework with gas sorption properties and high adsorptive selectivity for light hydrocarbons
Jia Li; Ying Guo; Hong-Ru Fu; Jian Zhang; Rong-Bin Huang; Lan-Sun Zheng; Jun Tao; Chem.Commun. 50 (2014) 9161–; doi:10.1039/C4cc02396J

data_7115427
_publ_section_title
;
 A spin-canted NiII4-based metal-organic framework with gas sorption
 properties and high adsorptive selectivity for light hydrocarbons
;
_journal_name_full               Chem.Commun.
_journal_page_first              9161
_journal_paper_doi               10.1039/C4cc02396J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C30 H30 N4 Ni4 O17'
_chemical_formula_sum            'C30 H30 N4 Ni4 O17'
_chemical_formula_weight         953.42
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-31
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.497(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8539(5)
_cell_length_b                   14.4578(8)
_cell_length_c                   30.4530(17)
_cell_measurement_temperature    100.01(10)
_cell_volume                     5623.0(5)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0591
_diffrn_reflns_av_unetI/netI     0.0888
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            28515
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_platon_squeeze_details
;
;
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         11013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                7861
_reflns_number_total             11013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc02396j2.cif
_cod_data_source_block           1S
_cod_database_code               7115427
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
2.b Ternary CH refined with riding coordinates:
 O13(H13), O14(H14)
2.c Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
2.d Aromatic/amide H refined with riding coordinates:
 C25(H25), C28(H28), C3(H3), C23(H23), C22(H22), C29(H29), C12(H12), C19(H19),
 C20(H20), C26(H26)
;