In situ variable-temperature single crystal X-ray diffraction studies of the single-crystal-to-single-crystal dehydration and rehydration of a mixed-ligand 2D zinc metal‒organic framework using trimesate and 4,4′-bipyridine-N,N′-dioxide as ligands
Tahier, Tayyibah; Oliver, Clive L.; CrystEngComm 17 (2015) 8946–; doi:10.1039/C5CE01297J

data_7221983
_publ_section_title
;
 In situ variable-temperature single crystal X-ray diffraction studies of
 the single-crystal-to-single-crystal dehydration and rehydration of a
 mixed-ligand 2D zinc metal--organic framework using trimesate and
 4,4&#x2032;-bipyridine-N,N&#x2032;-dioxide as ligands
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8946
_journal_paper_doi               10.1039/C5CE01297J
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C57 H54 N6 O48 S3 Zn9, 3(H2 O), 4(O)'
_chemical_formula_sum            'C57 H60 N6 O55 S3 Zn9'
_chemical_formula_weight         2393.62
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-15 deposited with the CCDC.
2015-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.816(4)
_cell_length_b                   18.816(4)
_cell_length_c                   21.441(5)
_cell_measurement_reflns_used    670
_cell_measurement_temperature    104
_cell_measurement_theta_max      23.957
_cell_measurement_theta_min      2.327
_cell_volume                     6574(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      104
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19838
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.668
_diffrn_reflns_theta_min         2.165
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.598
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             3606
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.317
_refine_diff_density_max         2.490
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 3400 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7900
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0546P)^2^+29.2088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.906
_reflns_friedel_fraction_full    0.990
_reflns_friedel_fraction_max     0.847
_reflns_number_gt                7628
_reflns_number_total             7900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01297j2.cif
_cod_data_source_block           104k
_cod_depositor_comments
'Adding full bibliography for 7221983--7221988.cif.'
_cod_database_code               7221983
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.820(2) 0.180(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O9-H9
 0.86 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O6WB)=1-FVAR(1)
 Sof(O6WA)=FVAR(1)
7.a Free rotating group:
 O4W(H4WA,H4WB)
7.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
7.c Ternary CH refined with riding coordinates:
 O9(H9)
7.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C16(H16), C2(H2), C10(H10), C6(H6), C13(H13), C4(H4), C19(H19),
 C17(H17), C14(H14), C18(H18)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id '104K '
_olex2_submission_special_instructions 'No special instructions were received'