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_4344412
_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         '0.5(C232 H216 N96 Ni16)'
_chemical_formula_sum            'C116 H108 N48 Ni8'
_chemical_formula_weight         2644.18
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-05
_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                 113.247(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.1753(12)
_cell_length_b                   23.1502(11)
_cell_length_c                   21.2350(18)
_cell_measurement_reflns_used    6001
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1930
_cell_measurement_theta_min      3.4310
_cell_volume                     7757.8(11)
_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-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4098
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0919
_diffrn_reflns_av_unetI/netI     0.1751
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31749
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.84
_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    1.003
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.802
_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            green
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-like
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0686
_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^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                6667
_reflns_number_total             13637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01844_si_002.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 4344404--4344414.cif.'
_cod_original_cell_volume        7757.8(9)
_cod_database_code               4344412
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H6A,H6B} of C6, {H13A,H13B} of C13, {H30A,H30B} of C30,
  {H37A,H37B} of C37, {H48A,H48B} of C48
 At 1.5 times of:
  All C(H,H,H) groups, {H24A,H24B} of C24
2.a Riding coordinates:
 C1(H1), C4(H4A,H4B,H4C), C5(H5), C6(H6A,H6B), C8(H8), C9(H9), C10(H10),
 C12(H12), C13(H13A,H13B), C14(H14), C16(H16), C18(H18A,H18B,H18C), C19(H19),
 C22(H22A,H22B,H22C), C23(H23), C24(H24A,H24B), C25(H25), C28(H28A,H28B,H28C),
 C29(H29), C30(H30A,H30B), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37A,
 H37B), C38(H38), C41(H41), C42(H42A,H42B,H42C), C43(H43), C46(H46A,H46B,H46C),
 C47(H47), C48(H48A,H48B), C50(H50), C52(H52), C53(H53), C54(H54)
;
_olex2_computing_structure_refinement_long 'ShelXL-1997 (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'