A series of oxyfluoride chains containing asymmetric basic building units of both early- and late-transition metal cations
Belal Ahmed; Hongil Jo; Sung Won Yoon; Kwang Yong Choi; Kang Min Ok; Journal of Solid State Chemistry 267 (2018) 140–145; doi:10.1016/j.jssc.2018.08.021

data_1560778
_publ_section_title
;
 A series of oxyfluoride chains containing asymmetric basic building units
 of both early- and late-transition metal cations
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              140
_journal_page_last               145
_journal_paper_doi               10.1016/j.jssc.2018.08.021
_journal_volume                  267
_journal_year                    2018
_chemical_formula_moiety         'C12 H16 F4 N8 Ni O2 W'
_chemical_formula_sum            'C12 H16 F4 N8 Ni O2 W'
_chemical_formula_weight         622.89
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.61(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.239(3)
_cell_length_b                   12.290(3)
_cell_length_c                   15.440(4)
_cell_measurement_reflns_used    6407
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.6
_cell_measurement_wavelength     0.71073
_cell_volume                     1930.0(9)
_computing_cell_refinement       'SAINT V7.68A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'Bruker APEX2 software'
_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      296(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.011479
_diffrn_orient_matrix_UB_12      0.00521
_diffrn_orient_matrix_UB_13      0.06512
_diffrn_orient_matrix_UB_21      0.109088
_diffrn_orient_matrix_UB_22      0.084522
_diffrn_orient_matrix_UB_23      0.001578
_diffrn_orient_matrix_UB_31      -0.065315
_diffrn_orient_matrix_UB_32      0.095436
_diffrn_orient_matrix_UB_33      0.00279
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20100
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         2.599
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    6.994
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.724
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00489(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0303P)^2^+7.8817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.069
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0
_reflns_number_gt                1936
_reflns_number_total             2401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-267-140.cif
_cod_data_source_block           4
_cod_original_cell_volume        1929.9(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1560778
_shelx_estimated_absorpt_t_min   0.33
_shelx_estimated_absorpt_t_max   0.359