Fine Tuning and Specific Binding Sites with a Porous Hydrogen-Bonded Metal-Complex Framework for Gas Selective Separations.
Bao, Zongbi; Xie, Danyan; Chang, Ganggang; Wu, Hui; Li, Liangying; Zhou, Wei; Wang, Hailong; Zhang, Zhiguo; Xing, Huabin; Yang, Qiwei; Zaworotko, Michael J.; Ren, Qilong; Chen, Banglin; Journal of the American Chemical Society 140 (2018) 4596–4603; doi:10.1021/jacs.7b13706

data_4131998
_publ_section_title
;
 Fine Tuning and Specific Binding Sites with a Porous Hydrogen-Bonded
 Metal-Complex Framework for Gas Selective Separations.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4596
_journal_page_last               4603
_journal_paper_doi               10.1021/jacs.7b13706
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C20 H24 Cu2 N20 O2, 2(F6 Si)'
_chemical_formula_sum            'C20 H24 Cu2 F12 N20 O2 Si2'
_chemical_formula_weight         987.85
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9982(8)
_cell_length_b                   11.0287(5)
_cell_length_c                   21.3180(11)
_cell_measurement_reflns_used    3475
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1059
_cell_measurement_theta_min      2.9095
_cell_volume                     3996.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0187031000
_diffrn_orient_matrix_UB_12      -0.0267706000
_diffrn_orient_matrix_UB_13      -0.0263155000
_diffrn_orient_matrix_UB_21      -0.0124493000
_diffrn_orient_matrix_UB_22      -0.0491517000
_diffrn_orient_matrix_UB_23      0.0190265000
_diffrn_orient_matrix_UB_31      -0.0351489000
_diffrn_orient_matrix_UB_32      0.0317051000
_diffrn_orient_matrix_UB_33      0.0072654000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12448
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
;
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0774P)^2^+8.8562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                1581
_reflns_number_total             1941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b13706_si_002.cif
_cod_data_source_block           160111_xdy_mpmf
_cod_database_code               4131998
_chemical_oxdiff_formula         'C10 H10 N2 O8 F1 Cu1'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
3.a Rotating group:
 O1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C4(H4)
3.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
;