Analysis of rapidly synthesized guest-filled porous complexes with synchrotron radiation: practical guidelines for the crystalline sponge method
Ramadhar, Timothy R.; Zheng, Shao-Liang; Chen, Yu-Sheng; Clardy, Jon; Acta Crystallographica Section A 71 (2015) –; doi:10.1107/S2053273314019573

data_2310149
_publ_section_title
;
 Analysis of rapidly synthesized guest-filled porous complexes with
 synchrotron radiation: practical guidelines for the crystalline sponge
 method
;
_journal_coeditor_code           PC5042
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053273314019573
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'C36 H24 I6 N12 Zn3, 2.44(C10 H12 O)'
_chemical_formula_sum            'C60.41 H53.29 I6 N12 O2.44 Zn3'
_chemical_formula_weight         1943.90
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4150(13)
_cell_angle_gamma                90
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_cell_length_a                   34.346(2)
_cell_length_b                   15.1140(9)
_cell_length_c                   32.5502(19)
_cell_measurement_reflns_used    9280
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.245
_cell_measurement_theta_min      2.233
_cell_volume                     16436.0(17)
_computing_cell_refinement       'SAINT 8.32B (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 v2014.3 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT 8.32B (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL XT-2014 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41317
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            118509
_diffrn_reflns_theta_full        14.353
_diffrn_reflns_theta_max         14.252
_diffrn_reflns_theta_min         0.709
_exptl_absorpt_coefficient_mu    1.675
_exptl_absorpt_correction_T_max  0.9279
_exptl_absorpt_correction_T_min  0.8251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1148 before and 0.0878 after correction. The Ratio of minimum to maximum transmission is 0.8892. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       prism
_exptl_crystal_F_000             7418
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.545
_refine_diff_density_min         -2.502
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         13986
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1800P)^2^+250.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2588
_reflns_number_gt                12328
_reflns_number_total             13986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pc5042sup1.cif
_cod_data_source_block           transanethole_a
_cod_original_cell_volume        16436.1(17)
_cod_database_code               2310149
_cod_database_fobs_code          2310149
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.906
_shelx_hkl_checksum              57138
_shelx_res_checksum              26824
_shelxl_version_number           201.4