Improvements to the Practical Usability of the "Crystalline Sponge" Method for Organic Structure Determination.
Waldhart, Greyson W.; Mankad, Neal P.; Santarsiero, Bernard D.; Organic letters 18 (2016) 6112–6115; doi:10.1021/acs.orglett.6b03119

data_1555942
_publ_section_title
;
 Improvements to the Practical Usability of the &quot;Crystalline
 Sponge&quot; Method for Organic Structure Determination.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              6112
_journal_page_last               6115
_journal_paper_doi               10.1021/acs.orglett.6b03119
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C36 H24 I6 N12 Zn3, 2.070(C12 H19 N)'
_chemical_formula_sum            'C60.84 H63.33 I6 N14.07 Zn3'
_chemical_formula_weight         1949.15
_chemical_name_common            'ZnI tris(4-pyridyl)-1,3,5-triazene)2 MOF'
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.234(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.538(6)
_cell_length_b                   14.7160(10)
_cell_length_c                   30.585(6)
_cell_measurement_reflns_used    144656
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.280
_cell_measurement_theta_min      1.137
_cell_volume                     16072(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'MAR 300mm CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70845
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            139756
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.155
_diffrn_reflns_theta_max         28.098
_diffrn_reflns_theta_min         1.358
_diffrn_source                   'APS 21-ID-D'
_exptl_absorpt_coefficient_mu    3.176
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS local scalinlg'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             7479
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.412
_refine_diff_density_min         -2.476
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.00072(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         19652
_refine_ls_number_restraints     561
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.0916
_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^)+(0.0578P)^2^+553.0012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12947
_reflns_number_total             19652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03119_si_003.cif
_cod_data_source_block           dipab
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1555942
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              77886
_shelx_hkl_checksum              48598