Fluoride-Rich, Hydrofluorothermal Routes to Functional Transition Metal (Mn, Fe, Co, Cu) Fluorophosphates
Jennifer A. Armstrong; Edward R. Williams; Mark T. Weller; Journal of the American Chemical Society 133 (2011) 8252–8263; doi:10.1021/ja201096b

data_4106164
_publ_section_title
;
 Fluoride-Rich, Hydrofluorothermal Routes to Functional Transition Metal
 (Mn, Fe, Co, Cu) Fluorophosphates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8252
_journal_page_last               8263
_journal_paper_doi               10.1021/ja201096b
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C20.4 Co4 F O24.04 P6'
_chemical_formula_weight         1070.18
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-01-11 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9197(3)
_cell_length_b                   12.9197(3)
_cell_length_c                   9.8491(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     1644.00(9)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11690
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  0.9753
_exptl_absorpt_correction_T_min  0.4325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_F_000             903
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.542
_refine_ls_shift/su_mean         0.050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+13.2487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1796
_reflns_number_gt                1388
_reflns_number_total             1842
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja201096b_si_001.cif
_cod_data_source_block           2010jaa0117pbar4n2
_cod_original_sg_symbol_Hall     'P -4 -2 n'
_cod_database_code               4106164