Solvothermal Subcomponent Self-Assembly of Cubic Metal-Imidazolate Cages and Their Coordination Polymers.
Luo, Dong; Zhou, Xiao-Ping; Li, Dan; Inorganic chemistry 54 (2015) 10822–10828; doi:10.1021/acs.inorgchem.5b01844

data_4344413
_publ_section_title
;
 Solvothermal Subcomponent Self-Assembly of Cubic Metal-Imidazolate Cages
 and Their Coordination Polymers.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10822
_journal_page_last               10828
_journal_paper_doi               10.1021/acs.inorgchem.5b01844
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C116 H108 N42 Ni8, 2(Cl O4), 0.17(H12.24 O6)'
_chemical_formula_sum            'C116 H110 Cl2 N42 Ni8 O9'
_chemical_formula_weight         2777.04
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.1763(5)
_cell_length_b                   15.1763(5)
_cell_length_c                   47.0687(7)
_cell_measurement_reflns_used    7089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1930
_cell_measurement_theta_min      3.4310
_cell_volume                     9388.5(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            6336
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        50
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.8
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             4290
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2516
_refine_ls_wR_factor_ref         0.3006
_reflns_number_gt                1659
_reflns_number_total             3657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01844_si_002.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 4344404--4344414.cif.'
_cod_database_code               4344413
_olex2_refinement_description
;
1. Others
 Fixed Sof: H1WA(0.17) H1WB(0.17)
 Fixed U13: Ni1(0) C20(0) O1(0) Cl1(0)
 Fixed U23: Ni1(0) C20(0) O1(0) Cl1(0)
 Fixed Uiso: H1(0.145) H3(0.118) H5(0.15) H6(0.174) H7A(0.13) H7B(0.13)
 H8(0.106) H10(0.091) H11A(0.172) H11B(0.172) H11C(0.172) H13A(0.175)
 H13B(0.175) H13C(0.175) H16(0.09) H17(0.142) H18A(0.141) H18B(0.141)
 H1WA(0.777) H1WB(0.777)
 Fixed X: Ni1(1) H1(0.7329) H3(0.7798) H5(0.5013) H6(0.5637) H7A(0.5952)
 H7B(0.5222) H8(0.7244) H10(0.7989) H11A(0.4906) H11B(0.4692) H11C(0.5627)
 H13A(0.606) H13B(0.5525) H13C(0.5895) H16(0.8625) H17(1.2507) H18A(1.234)
 H18B(1.1299) C20(0.3333) O1(0.6667) Cl1(0.6667) O1W(1) H1WA(1.0383)
 H1WB(1.0361)
 Fixed Y: Ni1(1) H1(0.8943) H3(1.1001) H5(0.8588) H6(0.806) H7A(1.0855)
 H7B(0.9744) H8(1.1925) H10(1.0668) H11A(0.8487) H11B(0.854) H11C(0.9461)
 H13A(0.6851) H13B(0.7442) H13C(0.6911) H16(1.032) H17(1.028) H18A(1.1064)
 H18B(1.1056) C20(0.6667) O1(0.3333) Cl1(0.3333) O1W(1) H1WA(1.0199)
 H1WB(1.0228)
 Fixed Z: H1(0.1768) H3(0.1155) H5(0.127) H6(0.1642) H7A(0.1014) H7B(0.0916)
 H8(0.0733) H10(-0.0187) H11A(-0.0449) H11B(-0.0125) H11C(-0.0271) H13A(0.0996)
 H13B(0.0887) H13C(0.067) H16(0.058) H17(0.1331) H18A(0.1668) H18B(0.1706)
 O1W(0) H1WA(-0.0145) H1WB(0.0149)
;
_olex2_computing_structure_refinement_long 'ShelXL-1997 (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS-1997 (Sheldrick, 2008)'