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_2310150
_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, 1.26(C15 H18), 0.7(C H Cl3)'
_chemical_formula_sum            'C55.61 H47.39 Cl2.1 I6 N12 Zn3'
_chemical_formula_weight         1915.66
_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                 102.8570(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.936(3)
_cell_length_b                   14.9785(13)
_cell_length_c                   30.825(3)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.252
_cell_measurement_theta_min      2.259
_cell_volume                     15726(2)
_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(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.957
_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     0.41321
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            91818
_diffrn_reflns_theta_full        14.355
_diffrn_reflns_theta_max         14.265
_diffrn_reflns_theta_min         0.863
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.6987
_exptl_absorpt_correction_T_min  0.5380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1617 before and 0.0687 after correction. The Ratio of minimum to maximum transmission is 0.7700. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       prism
_exptl_crystal_F_000             7270
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.279
_refine_diff_density_min         -1.912
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         13364
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0800P)^2^+550.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2392
_reflns_number_gt                12388
_reflns_number_total             13364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pc5042sup1.cif
_cod_data_source_block           guaiazulene_a
_cod_original_formula_sum        'C55.61 H47.39 Cl2.10 I6 N12 Zn3'
_cod_database_code               2310150
_cod_database_fobs_code          2310150
_shelx_estimated_absorpt_t_min   0.469
_shelx_estimated_absorpt_t_max   0.814
_shelx_hkl_checksum              91266
_shelx_res_checksum              97650
_shelxl_version_number           201.4