#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:47:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179394 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/91/4329193.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4329193
loop_
_publ_author_name
'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'
_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/[σ²(Fo²)+(0.0415P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zr1 Zr 0.5000 0.5000 0.5000 0.01457(12) Uani 1 2 d S
Cl1 Cl 0.37611(9) 0.48966(4) 0.63426(5) 0.0214(2) Uani 1 1 d .
Cl3 Cl 0.44022(9) 0.37902(4) 0.45837(5) 0.0216(2) Uani 1 1 d .
Cl2 Cl 0.27963(9) 0.53815(4) 0.40831(5) 0.0213(2) Uani 1 1 d .
P1 P 0.15919(9) 0.80535(4) 0.43398(6) 0.0167(2) Uani 1 1 d .
C1 C 0.0165(3) 0.85602(16) 0.3768(2) 0.0170(7) Uani 1 1 d .
C2 C -0.0528(3) 0.90317(16) 0.4251(2) 0.0207(8) Uani 1 1 d .
H2 H -0.0188 0.9120 0.4869 0.025 Uiso 1 1 calc R
C3 C -0.1718(4) 0.93721(18) 0.3827(2) 0.0263(8) Uani 1 1 d .
H3 H -0.2195 0.9697 0.4153 0.032 Uiso 1 1 calc R
C4 C -0.2209(4) 0.92381(18) 0.2929(2) 0.0261(8) Uani 1 1 d .
H4 H -0.3035 0.9466 0.2642 0.031 Uiso 1 1 calc R
C5 C -0.1509(4) 0.87750(18) 0.2447(2) 0.0244(8) Uani 1 1 d .
H5 H -0.1847 0.8691 0.1828 0.029 Uiso 1 1 calc R
C6 C -0.0324(4) 0.84356(17) 0.2860(2) 0.0221(8) Uani 1 1 d .
H6 H 0.0159 0.8118 0.2527 0.027 Uiso 1 1 calc R
C7 C 0.2909(3) 0.79128(17) 0.3620(2) 0.0180(7) Uani 1 1 d .
C8 C 0.3223(4) 0.84311(18) 0.3032(2) 0.0242(8) Uani 1 1 d .
H8 H 0.2673 0.8842 0.2975 0.029 Uiso 1 1 calc R
C9 C 0.4319(4) 0.83534(19) 0.2536(2) 0.0272(8) Uani 1 1 d .
H9 H 0.4512 0.8704 0.2127 0.033 Uiso 1 1 calc R
C10 C 0.5145(4) 0.77613(19) 0.2635(2) 0.0276(9) Uani 1 1 d .
H10 H 0.5912 0.7710 0.2298 0.033 Uiso 1 1 calc R
C11 C 0.4856(4) 0.72456(18) 0.3222(2) 0.0229(8) Uani 1 1 d .
H11 H 0.5425 0.6841 0.3289 0.027 Uiso 1 1 calc R
C12 C 0.3735(4) 0.73195(17) 0.3713(2) 0.0215(8) Uani 1 1 d .
H12 H 0.3532 0.6964 0.4114 0.026 Uiso 1 1 calc R
C13 C 0.2404(3) 0.84861(17) 0.5339(2) 0.0196(8) Uani 1 1 d .
C14 C 0.1837(4) 0.84269(18) 0.6142(2) 0.0252(8) Uani 1 1 d .
H14 H 0.1002 0.8162 0.6159 0.030 Uiso 1 1 calc R
C15 C 0.2479(4) 0.87515(19) 0.6917(2) 0.0304(9) Uani 1 1 d .
H15 H 0.2086 0.8710 0.7464 0.036 Uiso 1 1 calc R
C16 C 0.3686(4) 0.91337(19) 0.6895(3) 0.0339(10) Uani 1 1 d .
H16 H 0.4136 0.9347 0.7433 0.041 Uiso 1 1 calc R
C17 C 0.4257(4) 0.92121(19) 0.6100(3) 0.0326(9) Uani 1 1 d .
H17 H 0.5084 0.9484 0.6089 0.039 Uiso 1 1 calc R
C18 C 0.3609(4) 0.88893(17) 0.5318(2) 0.0246(8) Uani 1 1 d .
H18 H 0.3989 0.8944 0.4768 0.030 Uiso 1 1 calc R
C19 C 0.0882(3) 0.72544(16) 0.4680(2) 0.0181(7) Uani 1 1 d .
C20 C 0.1635(4) 0.68613(17) 0.5366(2) 0.0215(8) Uani 1 1 d .
H20 H 0.2539 0.7012 0.5650 0.026 Uiso 1 1 calc R
C21 C 0.1064(4) 0.62503(18) 0.5634(2) 0.0281(9) Uani 1 1 d .
H21 H 0.1581 0.5980 0.6099 0.034 Uiso 1 1 calc R
C22 C -0.0253(4) 0.60328(18) 0.5230(2) 0.0291(9) Uani 1 1 d .
H22 H -0.0651 0.5619 0.5426 0.035 Uiso 1 1 calc R
C23 C -0.0995(4) 0.64177(18) 0.4539(2) 0.0267(9) Uani 1 1 d .
H23 H -0.1896 0.6264 0.4255 0.032 Uiso 1 1 calc R
C24 C -0.0427(4) 0.70242(17) 0.4264(2) 0.0232(8) Uani 1 1 d .
H24 H -0.0937 0.7285 0.3786 0.028 Uiso 1 1 calc R
N1 N 0.2215(4) 0.47702(17) 0.8985(2) 0.0436(9) Uani 1 1 d .
C25 C 0.1542(4) 0.46956(19) 0.8304(3) 0.0296(9) Uani 1 1 d .
C26 C 0.0680(4) 0.4588(2) 0.7429(2) 0.0335(9) Uani 1 1 d .
H26A H 0.0468 0.4095 0.7346 0.050 Uiso 1 1 calc R
H26B H 0.1200 0.4749 0.6949 0.050 Uiso 1 1 calc R
H26C H -0.0208 0.4847 0.7405 0.050 Uiso 1 1 calc R
N2 N 0.1432(4) 0.29533(18) 0.8255(3) 0.0522(11) Uani 1 1 d .
C27 C 0.2207(4) 0.29607(19) 0.8897(3) 0.0347(10) Uani 1 1 d .
C28 C 0.3183(4) 0.2970(2) 0.9735(3) 0.0373(10) Uani 1 1 d .
H28A H 0.3243 0.3439 0.9983 0.056 Uiso 1 1 calc R
H28B H 0.4123 0.2821 0.9619 0.056 Uiso 1 1 calc R
H28C H 0.2841 0.2655 1.0170 0.056 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl2 Zr1 Cl2 180.0 . 3_666
Cl2 Zr1 Cl3 89.79(3) . .
Cl2 Zr1 Cl3 90.21(3) 3_666 .
Cl2 Zr1 Cl3 90.21(3) . 3_666
Cl2 Zr1 Cl3 89.79(3) 3_666 3_666
Cl3 Zr1 Cl3 180.0 . 3_666
Cl2 Zr1 Cl1 90.50(3) . .
Cl2 Zr1 Cl1 89.50(3) 3_666 .
Cl3 Zr1 Cl1 90.47(3) . .
Cl3 Zr1 Cl1 89.53(3) 3_666 .
Cl2 Zr1 Cl1 89.50(3) . 3_666
Cl2 Zr1 Cl1 90.50(3) 3_666 3_666
Cl3 Zr1 Cl1 89.53(3) . 3_666
Cl3 Zr1 Cl1 90.47(3) 3_666 3_666
Cl1 Zr1 Cl1 180.0 . 3_666
C7 P1 C13 108.48(15) . .
C7 P1 C19 111.40(15) . .
C13 P1 C19 107.66(16) . .
C7 P1 C1 110.23(15) . .
C13 P1 C1 110.55(15) . .
C19 P1 C1 108.50(15) . .
C2 C1 C6 120.2(3) . .
C2 C1 P1 119.8(2) . .
C6 C1 P1 119.8(3) . .
C3 C2 C1 119.6(3) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
C4 C3 C2 119.8(3) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C5 C4 C3 120.5(3) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C6 C5 C4 120.2(3) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C1 119.6(3) . .
C5 C6 H6 120.2 . .
C1 C6 H6 120.2 . .
C12 C7 C8 119.3(3) . .
C12 C7 P1 120.2(3) . .
C8 C7 P1 120.1(3) . .
C9 C8 C7 120.6(3) . .
C9 C8 H8 119.7 . .
C7 C8 H8 119.7 . .
C8 C9 C10 119.8(3) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C11 C10 C9 120.2(3) . .
C11 C10 H10 119.9 . .
C9 C10 H10 119.9 . .
C10 C11 C12 120.0(3) . .
C10 C11 H11 120.0 . .
C12 C11 H11 120.0 . .
C11 C12 C7 120.0(3) . .
C11 C12 H12 120.0 . .
C7 C12 H12 120.0 . .
C14 C13 C18 119.3(3) . .
C14 C13 P1 120.5(3) . .
C18 C13 P1 120.2(3) . .
C15 C14 C13 120.4(4) . .
C15 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
C16 C15 C14 119.9(4) . .
C16 C15 H15 120.1 . .
C14 C15 H15 120.1 . .
C15 C16 C17 120.8(4) . .
C15 C16 H16 119.6 . .
C17 C16 H16 119.6 . .
C16 C17 C18 119.4(4) . .
C16 C17 H17 120.3 . .
C18 C17 H17 120.3 . .
C17 C18 C13 120.1(3) . .
C17 C18 H18 119.9 . .
C13 C18 H18 119.9 . .
C24 C19 C20 119.4(3) . .
C24 C19 P1 120.2(3) . .
C20 C19 P1 120.4(3) . .
C21 C20 C19 119.9(3) . .
C21 C20 H20 120.1 . .
C19 C20 H20 120.1 . .
C22 C21 C20 120.3(3) . .
C22 C21 H21 119.8 . .
C20 C21 H21 119.8 . .
C21 C22 C23 119.9(3) . .
C21 C22 H22 120.0 . .
C23 C22 H22 120.0 . .
C24 C23 C22 120.1(3) . .
C24 C23 H23 120.0 . .
C22 C23 H23 120.0 . .
C23 C24 C19 120.4(3) . .
C23 C24 H24 119.8 . .
C19 C24 H24 119.8 . .
N1 C25 C26 179.1(4) . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
N2 C27 C28 178.8(5) . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 Cl2 2.4530(8) .
Zr1 Cl2 2.4530(8) 3_666
Zr1 Cl3 2.4699(8) .
Zr1 Cl3 2.4699(8) 3_666
Zr1 Cl1 2.4771(8) .
Zr1 Cl1 2.4771(8) 3_666
P1 C7 1.786(3) .
P1 C13 1.790(3) .
P1 C19 1.791(3) .
P1 C1 1.792(3) .
C1 C2 1.389(4) .
C1 C6 1.392(4) .
C2 C3 1.384(4) .
C2 H2 0.9500 .
C3 C4 1.383(5) .
C3 H3 0.9500 .
C4 C5 1.381(5) .
C4 H4 0.9500 .
C5 C6 1.375(4) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.389(4) .
C7 C8 1.394(4) .
C8 C9 1.373(5) .
C8 H8 0.9500 .
C9 C10 1.387(5) .
C9 H9 0.9500 .
C10 C11 1.383(5) .
C10 H10 0.9500 .
C11 C12 1.386(5) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.390(5) .
C13 C18 1.392(5) .
C14 C15 1.383(5) .
C14 H14 0.9500 .
C15 C16 1.372(5) .
C15 H15 0.9500 .
C16 C17 1.384(5) .
C16 H16 0.9500 .
C17 C18 1.392(5) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C24 1.387(4) .
C19 C20 1.392(4) .
C20 C21 1.385(5) .
C20 H20 0.9500 .
C21 C22 1.379(5) .
C21 H21 0.9500 .
C22 C23 1.384(5) .
C22 H22 0.9500 .
C23 C24 1.380(4) .
C23 H23 0.9500 .
C24 H24 0.9500 .
N1 C25 1.133(5) .
C25 C26 1.458(5) .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
N2 C27 1.125(5) .
C27 C28 1.451(5) .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C7 P1 C1 C2 -145.2(3)
C13 P1 C1 C2 -25.3(3)
C19 P1 C1 C2 92.5(3)
C7 P1 C1 C6 40.5(3)
C13 P1 C1 C6 160.4(3)
C19 P1 C1 C6 -81.7(3)
C6 C1 C2 C3 0.7(5)
P1 C1 C2 C3 -173.6(3)
C1 C2 C3 C4 0.3(5)
C2 C3 C4 C5 -1.0(5)
C3 C4 C5 C6 0.8(5)
C4 C5 C6 C1 0.1(5)
C2 C1 C6 C5 -0.9(5)
P1 C1 C6 C5 173.4(3)
C13 P1 C7 C12 88.1(3)
C19 P1 C7 C12 -30.3(3)
C1 P1 C7 C12 -150.8(3)
C13 P1 C7 C8 -84.7(3)
C19 P1 C7 C8 157.0(3)
C1 P1 C7 C8 36.5(3)
C12 C7 C8 C9 1.2(5)
P1 C7 C8 C9 174.0(3)
C7 C8 C9 C10 -1.5(5)
C8 C9 C10 C11 0.8(5)
C9 C10 C11 C12 0.1(5)
C10 C11 C12 C7 -0.4(5)
C8 C7 C12 C11 -0.3(5)
P1 C7 C12 C11 -173.1(2)
C7 P1 C13 C14 -154.9(3)
C19 P1 C13 C14 -34.2(3)
C1 P1 C13 C14 84.2(3)
C7 P1 C13 C18 25.5(3)
C19 P1 C13 C18 146.2(3)
C1 P1 C13 C18 -95.5(3)
C18 C13 C14 C15 -1.5(5)
P1 C13 C14 C15 178.9(3)
C13 C14 C15 C16 -0.1(5)
C14 C15 C16 C17 1.4(5)
C15 C16 C17 C18 -1.1(5)
C16 C17 C18 C13 -0.6(5)
C14 C13 C18 C17 1.9(5)
P1 C13 C18 C17 -178.5(3)
C7 P1 C19 C24 -101.6(3)
C13 P1 C19 C24 139.6(3)
C1 P1 C19 C24 19.9(3)
C7 P1 C19 C20 78.8(3)
C13 P1 C19 C20 -40.0(3)
C1 P1 C19 C20 -159.7(3)
C24 C19 C20 C21 -0.8(5)
P1 C19 C20 C21 178.8(3)
C19 C20 C21 C22 -0.6(5)
C20 C21 C22 C23 1.5(5)
C21 C22 C23 C24 -1.0(5)
C22 C23 C24 C19 -0.4(5)
C20 C19 C24 C23 1.3(5)
P1 C19 C24 C23 -178.3(3)
