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_2310151
_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
'C288 H192 I47.98 N96 Zn23.99, 10.21(C12 H22 O2), 0.55(C H Cl3)'
_chemical_formula_sum
'C411.01 H417.06 Cl1.65 I47.98 N96 O20.41 Zn23.99'
_chemical_formula_weight         14743.90
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.1910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   34.966(3)
_cell_length_b                   14.8683(14)
_cell_length_c                   66.990(6)
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.903
_cell_measurement_theta_min      2.273
_cell_volume                     33764(5)
_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 0.963
_diffrn_measured_fraction_theta_max 0.982
_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     0.41347
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            300285
_diffrn_reflns_theta_full        14.364
_diffrn_reflns_theta_max         14.258
_diffrn_reflns_theta_min         0.678
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0896 before and 0.0769 after correction. The Ratio of minimum to maximum transmission is 0.8759. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       prism
_exptl_crystal_F_000             14018
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.480
_refine_diff_density_min         -1.037
_refine_ls_abs_structure_details
;
 Flack x determined using 22730 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6312
_refine_ls_number_reflns         95898
_refine_ls_number_restraints     1137
_refine_ls_restrained_S_all      7.677
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+53.2554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1909
_reflns_number_gt                75484
_reflns_number_total             95898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pc5042sup1.cif
_cod_data_source_block           menthylacetate2_a
_cod_database_code               2310151
_cod_database_fobs_code          2310151
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.938
_shelx_hkl_checksum              33279
_shelx_res_checksum              60777
_shelxl_version_number           201.4