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_4106170
_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            'Cu3 F4 H8 N2 O12 P4'
_chemical_formula_weight         618.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-01-07 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.870(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8246(7)
_cell_length_b                   9.4940(8)
_cell_length_c                   9.1169(8)
_cell_measurement_reflns_used    21324
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     674.82(10)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7706
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    5.281
_exptl_absorpt_correction_T_max  0.6202
_exptl_absorpt_correction_T_min  0.6202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.044
_exptl_crystal_description       plate
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1549
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+9.6594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                1250
_reflns_number_total             1549
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja201096b_si_007.cif
_cod_data_source_block           2009erw0010mk1
_cod_database_code               4106170