Two interpenetrated metal‒organic frameworks with a slim ethynyl-based ligand: designed for selective gas adsorption and structural tuning
Kong, Xiang-Jing; Zhang, Yong-Zheng; He, Tao; Wu, Xue-Qian; Xu, Ming-Ming; Wang, Si-Nan; Xie, Lin-Hua; Li, Jian-Rong; CrystEngComm 20 (2018) 6018–; doi:10.1039/C8CE00779A

data_7230951
_publ_section_title
;
 Two interpenetrated metal--organic frameworks with a slim ethynyl-based
 ligand: designed for selective gas adsorption and structural tuning
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              6018
_journal_paper_doi               10.1039/C8CE00779A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '0.25(C168 H72 O64 Zr12)'
_chemical_formula_sum            'C42 H18 O16 Zr3'
_chemical_formula_weight         1052.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5470)
;
_audit_update_record
;
2018-05-10 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.068(5)
_cell_length_b                   42.667(2)
_cell_length_c                   13.8078(11)
_cell_measurement_reflns_used    1844
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.7240
_cell_measurement_theta_min      3.7850
_cell_volume                     14768(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -83.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.0386   19.0000    0.0000 127
  2 omega   23.00   56.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0386 -125.0000 -150.0000 33
  3 omega   28.00   71.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1479  -30.0000   30.0000 43
  4 omega   48.00   74.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1479  -30.0000  -60.0000 26
  5 omega   77.00  177.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1479   61.0000  120.0000 100
  6 omega   41.00  152.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1479  -15.0000   90.0000 111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0348961000
_diffrn_orient_matrix_UB_12      -0.0126121000
_diffrn_orient_matrix_UB_13      -0.0833704000
_diffrn_orient_matrix_UB_21      -0.0453262000
_diffrn_orient_matrix_UB_22      0.0222345000
_diffrn_orient_matrix_UB_23      0.0305968000
_diffrn_orient_matrix_UB_31      0.0222265000
_diffrn_orient_matrix_UB_32      0.0255419000
_diffrn_orient_matrix_UB_33      -0.0676509000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15455
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.526
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light colourless'
_exptl_crystal_density_diffrn    0.946
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         6978
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0711
_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^)+(0.1236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4028
_reflns_number_total             6978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00779a2.cif
_cod_data_source_block           BUT-44
_cod_depositor_comments
'Adding full bibliography for 7230951--7230952.cif.'
_cod_database_code               7230951
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O Zr'
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.661
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C17) \\sim
Ueq, Uanis(C19) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C16) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Zr1) \\sim Ueq, Uanis(Zr2) \\sim Ueq, Uanis(Zr3) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C3(H3), C4(H4), C7(H7), C17(H17), C19(H19), C6(H6), C18(H18),
 C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'