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_7226684
_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(C202.01 H122.02 N14 O54 Zn12)'
_chemical_formula_sum            'C101 H61.01 N7 O27 Zn6'
_chemical_formula_weight         2196.79
_chemical_name_systematic        UBMOF-3
_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   mixed
_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                 102.189(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   51.107(13)
_cell_length_b                   9.448(3)
_cell_length_c                   18.492(5)
_cell_measurement_reflns_used    2654
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.397
_cell_measurement_theta_min      0.815
_cell_volume                     8728(4)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.964
_diffrn_measured_fraction_theta_max 0.958
_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  0.1309
_diffrn_reflns_av_unetI/netI     0.1528
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27822
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_min         0.815
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.4895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1220 before and 0.0600 after correction. The Ratio of minimum to maximum transmission is 0.6571. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.836
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.183
_refine_diff_density_min         -2.237
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         8578
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.1054
_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^)+(0.1865P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2852
_refine_ls_wR_factor_ref         0.3082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5032
_reflns_number_total             8578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01783e2.cif
_cod_data_source_block           UBMOF-3
_cod_depositor_comments
'Adding full bibliography for 7226684--7226685.cif.'
_cod_database_code               7226684
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C26 \\sim N2-C25
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C18A) = Uiso(C19A) = Uiso(C20A) = Uiso(C21A) = Uiso(C22A) = Uiso(C23A)
Uiso(C18) = Uiso(C19) = Uiso(C23) = Uiso(C22) = Uiso(C21) = Uiso(C20)
Uiso(C15A) = Uiso(C14A) = Uiso(C13A) = Uiso(N1A) = Uiso(C17A) = Uiso(C16A)
Uiso(C15) = Uiso(C16) = Uiso(C17) = Uiso(N1) = Uiso(C13) = Uiso(C14)
Uanis(Zn1) = Uanis(Zn2)
Uanis(O1) = Uanis(C1) = Uanis(O2)
Uanis(C3) = Uanis(C4)
4. Others
 Sof(O7)=Sof(N2)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Fixed Sof: N1A(0.5) C17A(0.5) H17A(0.5) C16A(0.5) H16A(0.5) C15A(0.5)
 C14A(0.5) H14A(0.5) C13A(0.5) H13A(0.5) C15(0.5) C16(0.5) H16(0.5) C17(0.5)
 H17(0.5) N1(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5) C18(0.5) C19(0.5)
 C20(0.5) C21(0.5) C22(0.5) C23(0.5) C21A(0.5) C22A(0.5) C23A(0.5) C18A(0.5)
 C19A(0.5) C20A(0.5)
5.a Riding coordinates:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
5.b Aromatic/amide H refined with riding coordinates:
 C17A(H17A), C16A(H16A), C14A(H14A), C13A(H13A), C3(H3), C4(H4), C6(H6),
 C7(H7), C11(H11), C12(H12), C16(H16), C17(H17), C13(H13), C14(H14), C24(H24)
5.c Fitted hexagon refined as free rotating group:
 N1A(C17A,C16A,C15A,C14A,C13A), C15(C16,C17,N1,C13,C14), C18(C19,C20,C21,C22,
 C23), C21A(C22A,C23A,C18A,C19A,C20A)
;
_olex2_submission_special_instructions 'No special instructions were received'