Ternary transition-metal fluoride precursors for the fluorolytic sol-gel route: new insights into speciation and decomposition.
Kohl, J.; Wiedemann, D.; Troyanov, S. I.; Palamidis, E.; Lerch, M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13272–13281; doi:10.1039/c5dt01748c

data_7035538
_publ_section_title
;
 Ternary transition-metal fluoride precursors for the fluorolytic sol-gel
 route: new insights into speciation and decomposition.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13272
_journal_page_last               13281
_journal_paper_doi               10.1039/c5dt01748c
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Mn (C5 H5 N)3 F3]'
_chemical_formula_moiety         'C15 H15 F3 Mn N3'
_chemical_formula_sum            'C15 H15 F3 Mn N3'
_chemical_formula_weight         349.24
_chemical_name_systematic        mer-trifluoridotris(pyridine)manganese(III)
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   difmap
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_audit_update_record
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.981(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9240(19)
_cell_length_b                   8.1630(8)
_cell_length_c                   12.4914(13)
_cell_measurement_reflns_used    2304
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      31.4310
_cell_measurement_theta_min      3.6650
_cell_volume                     1582.2(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_UB_11      -0.0329125000
_diffrn_orient_matrix_UB_12      0.0421740000
_diffrn_orient_matrix_UB_13      -0.0375873000
_diffrn_orient_matrix_UB_21      0.0017021000
_diffrn_orient_matrix_UB_22      -0.0596938000
_diffrn_orient_matrix_UB_23      -0.0406761000
_diffrn_orient_matrix_UB_31      -0.0317418000
_diffrn_orient_matrix_UB_32      -0.0468849000
_diffrn_orient_matrix_UB_33      0.0180494000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5530
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.310
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.4486
_exptl_crystal_size_mid          0.3308
_exptl_crystal_size_min          0.2634
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5530
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1136P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.889
_reflns_friedel_fraction_full    0.891
_reflns_friedel_fraction_max     0.890
_reflns_number_gt                4185
_reflns_number_total             5530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01748c1.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7035533--7035539.cif.'
_cod_database_code               7035538
_shelx_shelxl_version_number     2014/7
_twin_formation_mechanism        gt
_twin_dimensionality             triperiodic
_twin_morphology                 simple
_twin_special_details
;       
Individuals are twinned by rotation of ca. 180\% around [-0.25 0 1] in
reciprocal or (0 0 1) in direct space.
;
_shelx_res_checksum              50992