Structural and spectroscopic studies of fluoroprotactinates.
De Sio, Stéphanie M; Wilson, Richard E.; Inorganic chemistry 53 (2014) 1750–1755; doi:10.1021/ic402877a

data_4337360
_publ_section_title
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 Structural and spectroscopic studies of fluoroprotactinates.
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_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1750
_journal_page_last               1755
_journal_paper_doi               10.1021/ic402877a
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'F7 Pa, 2(H4 N)'
_chemical_formula_sum            'F7 H8 N2 Pa'
_chemical_formula_weight         400.08
_chemical_melting_point          ?
_chemical_name_common            'diammonium heptafluoroprotactinate(V)'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.606(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1003(10)
_cell_length_b                   6.8966(9)
_cell_length_c                   11.8834(15)
_cell_measurement_reflns_used    8751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.51
_cell_volume                     663.82(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.5 deg w/ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8751
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    23.563
_exptl_absorpt_correction_T_max  0.1090
_exptl_absorpt_correction_T_min  0.0477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1909
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+0.7427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                1835
_reflns_number_total             1909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402877a_si_001.cif
_cod_data_source_block           NH4-PaF7
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
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_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4337360