Structural response to desolvation in a pyridyl-phenanthrene diarylethene-based metal‒organic framework
Walton, Ian M.; Cox, Jordan M.; Mitchell, Travis B.; Bizier, Nicholas P.; Benedict, Jason B.; CrystEngComm 18 (2016) 7972–; doi:10.1039/C6CE01783E

data_7226685
_publ_section_title
;
 Structural response to desolvation in a pyridyl-phenanthrene
 diarylethene-based metal--organic framework
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              7972
_journal_paper_doi               10.1039/C6CE01783E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.5(C224 H96 N8 O48 S8 Zn12)'
_chemical_formula_sum            'C112 H48 N4 O24 S4 Zn6'
_chemical_formula_weight         2354.00
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-30 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.374(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   39.751(4)
_cell_length_b                   9.7399(11)
_cell_length_c                   18.388(2)
_cell_measurement_reflns_used    2654
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.454
_cell_measurement_theta_min      2.050
_cell_volume                     7117.2(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28262
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.454
_diffrn_reflns_theta_min         2.050
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1263 before and 0.0546 after correction.
The Ratio of minimum to maximum transmission is 0.7470.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plate
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.987
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0790
_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^)+(0.1315P)^2^+20.3652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5051
_reflns_number_total             7293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01783e2.cif
_cod_data_source_block           UBMOF-3a
_cod_depositor_comments
'Adding full bibliography for 7226684--7226685.cif.'
_cod_original_cell_volume        7117.1(14)
_cod_database_code               7226685
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S1-C26 \\sim S1-C28 \\sim S1A-C26A \\sim S1A-C28A
 with sigma of 0.02
 C26-C25 \\sim C28-C27 \\sim C26A-C25A \\sim C28A-C27A
 with sigma of 0.02
 C27-C25 \\sim C27A-C25A
 with sigma of 0.02
3. Others
 Fixed Sof: S1(0.5) S1A(0.5) C24(0.5) C24A(0.5) C25(0.5) C25A(0.5) C26(0.5)
 C26A(0.5) C27(0.5) C27A(0.5) C28(0.5) C28A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14),
 C16(H16), C17(H17), C23(H23), C19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'