Two cyclohexane-type octadecanuclear metalla-macrocycle-based metal organic frameworks and adsorption properties
Chen, Shufang; Hu, Jiyong; Zhao, Jin'an; Zhang, Jin; Yu, Huaibin; Zhi, Shuangcheng; Zhang, Junshuai; Gong, Zhanqiang; CrystEngComm 18 (2016) 5353–; doi:10.1039/C6CE00494F

data_7225347
_publ_section_title
;
 Two cyclohexane-type octadecanuclear metalla-macrocycle-based metal
 organic frameworks and adsorption properties
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5353
_journal_paper_doi               10.1039/C6CE00494F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.02(C2208 H2112 N192 Ni48 O384 S96)'
_chemical_formula_sum            'C46 H44 N4 Ni O8 S2'
_chemical_formula_weight         903.68
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_Hall           '-I 4bd 2c 3'
_space_group_name_H-M_alt        'I a -3 d'
_symmetry_space_group_name_Hall  '-I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I a -3 d'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-01 deposited with the CCDC.
2016-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            48
_cell_length_a                   42.3668(2)
_cell_length_b                   42.3668(2)
_cell_length_c                   42.3668(2)
_cell_measurement_reflns_used    11616
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      73.5291
_cell_measurement_theta_min      3.2960
_cell_volume                     76046.1(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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      100.00(11)
_diffrn_detector_area_resol_mean 10.5281
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -23.00   31.00   1.0000   23.9300
omega____ theta____ kappa____ phi______ frames
    -      -40.4835   77.0000 -180.0000 54

  2 omega  137.00  163.00   1.0000  100.7100
omega____ theta____ kappa____ phi______ frames
    -      107.4530   77.0000 -180.0000 26

  3 omega  103.00  176.00   1.0000  100.7100
omega____ theta____ kappa____ phi______ frames
    -      107.4530   77.0000   90.0000 73
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0235845000
_diffrn_orient_matrix_UB_12      0.0249113000
_diffrn_orient_matrix_UB_13      0.0120888000
_diffrn_orient_matrix_UB_21      0.0007381000
_diffrn_orient_matrix_UB_22      -0.0152962000
_diffrn_orient_matrix_UB_23      0.0329826000
_diffrn_orient_matrix_UB_31      0.0276626000
_diffrn_orient_matrix_UB_32      0.0216211000
_diffrn_orient_matrix_UB_33      0.0094164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.691
_diffrn_reflns_theta_min         3.904
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.947
_exptl_crystal_description       block
_exptl_crystal_F_000             22656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6263
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2801
_refine_ls_wR_factor_ref         0.3084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4744
_reflns_number_total             6263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00494f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7225347--7225348.cif.'
_cod_original_cell_volume        76046.0(13)
_cod_database_code               7225347
_shelxl_version_number           2014-3
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-C1
 1.73 with sigma of 0.02
 C2-C1
 1.384 with sigma of 0.02
 C3-C2
 1.311 with sigma of 0.02
 C4-C3
 1.462 with sigma of 0.02
 S1-C4
 1.703 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C5(H5A,H5B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C8(H8), C10(H10), C22(H22), C21(H21), C3(H3), C1(H1),
 C2(H2)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'