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_2310152
_publ_section_title
;
 Analysis of rapidly synthesized guest-filled porous complexes with
 synchrotron radiation: practical guidelines for the crystalline sponge
 method
;
_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, 1.44(C H Cl3)'
_chemical_formula_sum            'C37.44 H25.44 Cl4.32 I6 N12 Zn3'
_chemical_formula_weight         1754.12
_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                 101.031(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.655(3)
_cell_length_b                   14.7307(14)
_cell_length_c                   31.081(3)
_cell_measurement_reflns_used    9406
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      14.219
_cell_measurement_theta_min      2.176
_cell_volume                     15573(3)
_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 0.959
_diffrn_measured_fraction_theta_max 0.976
_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     0.41333
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            115077
_diffrn_reflns_theta_full        14.359
_diffrn_reflns_theta_max         14.270
_diffrn_reflns_theta_min         0.876
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1419 before and 0.0669 after correction. The Ratio of minimum to maximum transmission is 0.8112. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       prism
_exptl_crystal_F_000             6524
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.382
_refine_diff_density_min         -2.884
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         13521
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0937
_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^)+(0.1800P)^2^+400.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2816
_refine_ls_wR_factor_ref         0.3384
_reflns_number_gt                10586
_reflns_number_total             13521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pc5042sup1.cif
_cod_data_source_block           znblank_a
_cod_original_cell_volume        15574(3)
_cod_database_code               2310152
_cod_database_fobs_code          2310152
_shelx_estimated_absorpt_t_min   0.619
_shelx_estimated_absorpt_t_max   0.930
_shelx_hkl_checksum              94232
_shelx_res_checksum              3413
_shelxl_version_number           201.4