Synthesis and Structure of (Ph4P)2MCl6 (M = Ti, Zr, Hf, Th, U, Np, Pu)
Stefan G. Minasian; Kevin S. Boland; Russell K. Feller; Andrew J. Gaunt; Stosh A. Kozimor; Iain May; Sean D. Reilly; Brian L. Scott; David K. Shuh; Inorganic Chemistry 51 (2012) 5728–5736; doi:10.1021/ic300179d

data_4329191
_publ_contact_author_address     'Los Alamos National Laboratory'
_publ_contact_author_email       stosh@lanl.gov
_publ_contact_author_name        'Stosh A. Kozimor'
_publ_contact_author_phone       505-665-4521
_publ_section_title
;
 Synthesis and Structure of (Ph4P)2MCl6 (M = Ti, Zr, Hf, Th, U, Np, Pu)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5728
_journal_page_last               5736
_journal_paper_doi               10.1021/ic300179d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C50 H43 F6 N P2 Ti'
_chemical_formula_weight         881.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.432(6)
_cell_angle_beta                 72.6920(10)
_cell_angle_gamma                79.405(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9307(16)
_cell_length_b                   10.5367(13)
_cell_length_c                   11.0318(16)
_cell_measurement_reflns_used    3905
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.28
_cell_volume                     1054.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10335
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.9347
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3830
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.7075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                3178
_reflns_number_total             3830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300179d_si_002_2.cif
_cod_data_source_block           apx919a
_cod_database_code               4329191