Expanded Porous Metal-Organic Frameworks by SCSC: Organic Building Units Modifying and Enhanced Gas-Adsorption Properties.
Fan, Weidong; Lin, Huan; Yuan, Xue; Dai, Fangna; Xiao, Zhenyu; Zhang, Liangliang; Luo, Liwen; Wang, Rongming; Inorganic chemistry 55 (2016) 6420–6425; doi:10.1021/acs.inorgchem.6b00278

data_4344889
_publ_section_title
;
 Expanded Porous Metal-Organic Frameworks by SCSC: Organic Building Units
 Modifying and Enhanced Gas-Adsorption Properties.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6420
_journal_page_last               6425
_journal_paper_doi               10.1021/acs.inorgchem.6b00278
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '0.13(C368 H216 Cu24 N32 O104)'
_chemical_formula_sum            'C46 H28 Cu3 N4 O13'
_chemical_formula_weight         1035.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.1668(10)
_cell_length_b                   34.1668(10)
_cell_length_c                   19.3425(9)
_cell_measurement_reflns_used    887
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.1880
_cell_measurement_theta_min      3.6480
_cell_volume                     22579.9(14)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  Cu
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.1364
_diffrn_reflns_av_unetI/netI     0.3225
_diffrn_reflns_Laue_measured_fraction_full 0.839
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21453
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.684
_exptl_absorpt_coefficient_mu    0.588
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.609
_exptl_crystal_description       block
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.636
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         9161
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.607
_refine_ls_R_factor_all          0.1930
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0430P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1636
_reflns_number_total             9161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00278_si_003.cif
_cod_data_source_block           exp_2773-sr
_cod_database_code               4344889
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C14-C14_$1 = C14-C14_$1
 1.45 with sigma of 0.01
 C14-C14_$1
 2.3 with sigma of 0.01
 C14-C14_$1
 2.2 with sigma of 0.01
 C13-C14
 2.2 with sigma of 0.01
 C13-C13
 1.43 with sigma of 0.01
 C14-C14
 1.43 with sigma of 0.01
 C13-C13_$1
 1.5 with sigma of 0.01
 C14-C14_$1 = C14-C14_$1
 1.5 with sigma of 0.01
 C14-C14_$1 = C14-C14_$1
 1.5 with sigma of 0.01
 C14-C14_$1 = C14-C14_$1
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.05 and sigma
for terminal atoms of 0.001
4. Others
 Sof(O0AB)=0.25*(1-FVAR(2))
 Sof(O0AA)=0.25*FVAR(2)
 Fixed Sof: H1(0.5)
5.a Rotating group:
 N1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C7(H7), C19(H19), C3(H3), C18(H18), C21(H21), C17(H17), C8(H8),
 C11(H11), C10(H10), C14(H14), C13(H13)
;
_shelx_res_checksum              2352
_shelx_hkl_checksum              70832
_olex2_submission_special_instructions 'No special instructions were received'