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_4329193
_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            'C56 H52 Cl6 N4 P2 Zr'
_chemical_formula_weight         1146.88
_chemical_name_systematic
; 
 ? 
;
_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                 98.159(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5282(12)
_cell_length_b                   19.366(2)
_cell_length_c                   14.9522(18)
_cell_measurement_reflns_used    1900
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      20.35
_cell_measurement_theta_min      2.40
_cell_volume                     2731.1(6)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1008
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28487
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.9652
_exptl_absorpt_correction_T_min  0.8146
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         6174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                3942
_reflns_number_total             6174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300179d_si_002_4.cif
_cod_data_source_block           apx1280
_cod_original_cell_volume        2731.2(6)
_cod_database_code               4329193