Hybrid materials based on transition Metal-BTC-Benzimidazole: Solvent assisted crystallographic and structural switching
Behera, Jogendra Nath; Tiwari, Ranjay K.; CrystEngComm  (2018) –; doi:10.1039/C8CE01299G

data_7231528
_publ_section_title
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 Hybrid materials based on transition Metal-BTC-Benzimidazole: Solvent
 assisted crystallographic and structural switching
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE01299G
_journal_year                    2018
_chemical_formula_moiety         'C25 H15 N3 O13 Zn2, 2(C7 H8 N3), 6(H2 O)'
_chemical_formula_sum            'C39 H43 N9 O19 Zn2'
_chemical_formula_weight         1072.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-09-21 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                97.411(2)
_cell_angle_beta                 102.378(2)
_cell_angle_gamma                105.892(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2050(3)
_cell_length_b                   14.3969(4)
_cell_length_c                   16.5940(4)
_cell_measurement_reflns_used    8753
_cell_measurement_temperature    296(2)
_cell_volume                     2244.14(11)
_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, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32668
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.416
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0667 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.8204.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             1104
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8250
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          2.550
_refine_ls_shift/su_mean         0.068
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.4726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6691
_reflns_number_total             8250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01299g2.cif
_cod_data_source_block           jnb_rt_2014_znbtc2abi
_cod_original_cell_volume        2244.13(11)
_cod_database_code               7231528
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O7W) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.05
Uanis(O3W) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.05
Uanis(O6W) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.05
Uanis(C35) \\sim Ueq: with sigma of 0.5 and sigma for terminal atoms of 0.05
3.a Free rotating group:
 O5W(H5WA,H5WB,O2W,H2WA,H2WB), O4W(H4WA,H4WB), O3W(H3WA,H3WB), O6W(H6WA,H6WB),
 O7W(H7WA,H7WB)
3.b Rotating group:
 O1W(H1WA,H1WB)
3.c Aromatic/amide H refined with riding coordinates:
 N4(H4A), C4(H4), N2(H2), C2(H2A), C15(H15), C13(H13), N6(H6A), N7(H7),
 C11(H11), C6(H6), C23(H23), N8(H8), C20(H20), C30(H30), C21(H21), C22(H22),
 C27(H27), C29(H29), C28(H28), C37(H37), C34(H34), C36(H36), C35(H35)
3.d X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N3(H3A,H3B), N9(H9A,H9B)
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_shelx_res_checksum              95505
_olex2_submission_special_instructions 'No special instructions were received'