Influence of structure-directing polyhedra and heterocyclic ligands on the chain structures and O/F ordering in a series of zinc vanadium oxyfluorides
Ahmed, Belal; Jo, Hongil; Lee, Suheon; Choi, Kwang-Yong; Ok, Kang Min; CrystEngComm  (2020) –; doi:10.1039/D0CE00318B

data_7240243
_publ_section_title
;
 Influence of structure-directing polyhedra and heterocyclic ligands on
 the chain structures and O/F ordering in a series of zinc vanadium
 oxyfluorides
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00318B
_journal_year                    2020
_chemical_formula_moiety         'C16 H26 F6 N8 O3 V2 Zn'
_chemical_formula_sum            'C16 H26 F6 N8 O3 V2 Zn'
_chemical_formula_weight         659.72
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-02-21 deposited with the CCDC.	2020-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.65(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.970(2)
_cell_length_b                   15.173(3)
_cell_length_c                   18.460(4)
_cell_measurement_reflns_used    56601
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_measurement_wavelength     0.63000
_cell_volume                     2689.0(10)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      297.85
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.63000
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29398
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.21
_diffrn_reflns_theta_max         26.741
_diffrn_reflns_theta_min         1.564
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.63
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.76
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     333
_refine_ls_number_reflns         8177
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+0.2904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                6302
_reflns_number_total             8177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00318b2.cif
_cod_data_source_block           ccompd_2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7240243
_shelx_estimated_absorpt_t_min   0.778
_shelx_estimated_absorpt_t_max   0.976