#------------------------------------------------------------------------------
#$Date: 2017-09-27 16:12:17 +0300 (Wed, 27 Sep 2017) $
#$Revision: 201370 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/77/4067724.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_4067724
loop_
_publ_author_name
'MacIntosh, Ian S.'
'Sherren, Cody N.'
'Robertson, Katherine N.'
'Masuda, Jason D.'
'Pye, Cory C.'
'Clyburne, Jason A. C.'
_publ_section_title
;
 Isolation and Structures of Two New Organozinc Anions from Solutions Rich
 in Halide Ions
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2063
_journal_paper_doi               10.1021/om901097r
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C48 H40 Cl4 P2 Zn'
_chemical_formula_weight         885.91
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.6220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9888(11)
_cell_length_b                   19.491(3)
_cell_length_c                   20.269(2)
_cell_measurement_reflns_used    4816
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.32
_cell_volume                     4339.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14306
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0367
_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)+(0.0520P)²+4.3474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                2989
_reflns_number_total             3818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901097r_si_001.cif
_cod_data_source_block           TPPZnCl4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4339.5(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4067724
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Zn1 Zn 0.5000 0.04407(2) 0.7500 0.05022(16) Uani 1 2 d S
P2 P 0.09178(6) 0.13276(4) 0.92395(4) 0.04682(19) Uani 1 1 d .
C17 C 0.2280(2) 0.10798(13) 0.96828(13) 0.0454(6) Uani 1 1 d .
C22 C 0.0813(3) -0.00370(14) 0.88622(14) 0.0509(7) Uani 1 1 d .
H22A H 0.1510 -0.0103 0.9125 0.061 Uiso 1 1 calc R
C23 C 0.0307(2) 0.06109(14) 0.87959(13) 0.0462(6) Uani 1 1 d .
C18 C 0.2180(3) 0.07279(17) 1.02747(15) 0.0610(8) Uani 1 1 d .
H18A H 0.1415 0.0637 1.0439 0.073 Uiso 1 1 calc R
C16 C 0.3421(3) 0.11978(15) 0.94378(14) 0.0544(7) Uani 1 1 d .
H16A H 0.3501 0.1424 0.9037 0.065 Uiso 1 1 calc R
C5 C 0.1213(3) 0.19960(14) 0.86567(14) 0.0520(7) Uani 1 1 d .
C11 C -0.0153(3) 0.16201(14) 0.98370(14) 0.0536(7) Uani 1 1 d .
C15 C 0.4442(3) 0.09787(16) 0.97905(16) 0.0623(8) Uani 1 1 d .
H15A H 0.5211 0.1060 0.9627 0.075 Uiso 1 1 calc R
C10 C -0.0568(4) 0.23376(17) 1.07647(18) 0.0799(11) Uani 1 1 d .
H10A H -0.0308 0.2660 1.1077 0.096 Uiso 1 1 calc R
C13 C 0.3206(3) 0.05143(17) 1.06180(16) 0.0661(8) Uani 1 1 d .
H13A H 0.3134 0.0281 1.1015 0.079 Uiso 1 1 calc R
C19 C 0.0276(3) -0.05832(16) 0.85347(16) 0.0647(8) Uani 1 1 d .
H19A H 0.0614 -0.1019 0.8575 0.078 Uiso 1 1 calc R
C6 C 0.1896(3) 0.18417(16) 0.81110(15) 0.0664(8) Uani 1 1 d .
H6A H 0.2186 0.1398 0.8052 0.080 Uiso 1 1 calc R
C24 C -0.0715(3) 0.07006(18) 0.83836(15) 0.0625(8) Uani 1 1 d .
H24A H -0.1041 0.1137 0.8321 0.075 Uiso 1 1 calc R
C20 C -0.1243(3) 0.0151(2) 0.80695(16) 0.0689(9) Uani 1 1 d .
H20A H -0.1936 0.0213 0.7802 0.083 Uiso 1 1 calc R
C14 C 0.4332(3) 0.06429(17) 1.03783(15) 0.0622(8) Uani 1 1 d .
H14A H 0.5025 0.0502 1.0615 0.075 Uiso 1 1 calc R
C12 C 0.0230(3) 0.20930(16) 1.03049(17) 0.0711(9) Uani 1 1 d .
H12A H 0.1030 0.2248 1.0311 0.085 Uiso 1 1 calc R
C4 C 0.0769(3) 0.26573(15) 0.87302(16) 0.0667(8) Uani 1 1 d .
H4A H 0.0314 0.2768 0.9095 0.080 Uiso 1 1 calc R
C21 C -0.0757(3) -0.04851(19) 0.81486(16) 0.0706(10) Uani 1 1 d .
H21A H -0.1128 -0.0858 0.7939 0.085 Uiso 1 1 calc R
C3 C 0.1003(4) 0.31491(16) 0.82626(18) 0.0773(10) Uani 1 1 d .
H3A H 0.0688 0.3589 0.8307 0.093 Uiso 1 1 calc R
C2 C 0.1696(4) 0.29924(18) 0.77334(19) 0.0805(10) Uani 1 1 d .
H2A H 0.1863 0.3329 0.7424 0.097 Uiso 1 1 calc R
C7 C -0.1332(3) 0.13799(18) 0.98425(17) 0.0681(9) Uani 1 1 d .
H7A H -0.1597 0.1055 0.9535 0.082 Uiso 1 1 calc R
C1 C 0.2145(4) 0.23422(19) 0.76572(17) 0.0805(10) Uani 1 1 d .
H1A H 0.2620 0.2240 0.7297 0.097 Uiso 1 1 calc R
C8 C -0.2119(3) 0.1625(2) 1.0309(2) 0.0876(12) Uani 1 1 d .
H8A H -0.2915 0.1464 1.0316 0.105 Uiso 1 1 calc R
C9 C -0.1727(4) 0.2106(2) 1.07584(19) 0.0867(12) Uani 1 1 d .
H9A H -0.2266 0.2276 1.1064 0.104 Uiso 1 1 calc R
Cl1 Cl 0.62629(7) -0.02315(4) 0.69109(4) 0.0661(2) Uani 1 1 d .
Cl3 Cl 0.39480(8) 0.11230(5) 0.67633(5) 0.0780(3) Uani 1 1 d .
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'
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'
Zn Zn 0.2839 1.4301 '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
Cl1 Zn1 Cl1 109.57(5) . 2_656
Cl1 Zn1 Cl3 107.28(3) . .
Cl1 Zn1 Cl3 111.91(3) 2_656 .
Cl1 Zn1 Cl3 111.92(3) . 2_656
Cl1 Zn1 Cl3 107.28(3) 2_656 2_656
Cl3 Zn1 Cl3 108.93(6) . 2_656
C23 P2 C17 109.84(12) . .
C23 P2 C5 108.03(13) . .
C17 P2 C5 111.22(13) . .
C23 P2 C11 110.04(13) . .
C17 P2 C11 107.48(13) . .
C5 P2 C11 110.25(13) . .
C16 C17 C18 119.2(3) . .
C16 C17 P2 122.0(2) . .
C18 C17 P2 118.8(2) . .
C19 C22 C23 119.5(3) . .
C19 C22 H22A 120.3 . .
C23 C22 H22A 120.3 . .
C22 C23 C24 119.2(3) . .
C22 C23 P2 121.4(2) . .
C24 C23 P2 119.4(2) . .
C13 C18 C17 120.2(3) . .
C13 C18 H18A 119.9 . .
C17 C18 H18A 119.9 . .
C17 C16 C15 119.7(3) . .
C17 C16 H16A 120.2 . .
C15 C16 H16A 120.2 . .
C6 C5 C4 119.1(3) . .
C6 C5 P2 118.7(2) . .
C4 C5 P2 122.2(2) . .
C7 C11 C12 119.3(3) . .
C7 C11 P2 122.0(2) . .
C12 C11 P2 118.7(2) . .
C14 C15 C16 120.6(3) . .
C14 C15 H15A 119.7 . .
C16 C15 H15A 119.7 . .
C9 C10 C12 119.6(4) . .
C9 C10 H10A 120.2 . .
C12 C10 H10A 120.2 . .
C14 C13 C18 120.3(3) . .
C14 C13 H13A 119.9 . .
C18 C13 H13A 119.9 . .
C21 C19 C22 120.2(3) . .
C21 C19 H19A 119.9 . .
C22 C19 H19A 119.9 . .
C1 C6 C5 120.2(3) . .
C1 C6 H6A 119.9 . .
C5 C6 H6A 119.9 . .
C20 C24 C23 120.4(3) . .
C20 C24 H24A 119.8 . .
C23 C24 H24A 119.8 . .
C21 C20 C24 120.0(3) . .
C21 C20 H20A 120.0 . .
C24 C20 H20A 120.0 . .
C13 C14 C15 120.1(3) . .
C13 C14 H14A 120.0 . .
C15 C14 H14A 120.0 . .
C11 C12 C10 120.5(3) . .
C11 C12 H12A 119.8 . .
C10 C12 H12A 119.8 . .
C3 C4 C5 120.0(3) . .
C3 C4 H4A 120.0 . .
C5 C4 H4A 120.0 . .
C20 C21 C19 120.7(3) . .
C20 C21 H21A 119.7 . .
C19 C21 H21A 119.7 . .
C2 C3 C4 120.2(3) . .
C2 C3 H3A 119.9 . .
C4 C3 H3A 119.9 . .
C3 C2 C1 120.4(3) . .
C3 C2 H2A 119.8 . .
C1 C2 H2A 119.8 . .
C11 C7 C8 119.6(3) . .
C11 C7 H7A 120.2 . .
C8 C7 H7A 120.2 . .
C2 C1 C6 120.1(3) . .
C2 C1 H1A 119.9 . .
C6 C1 H1A 119.9 . .
C9 C8 C7 120.0(4) . .
C9 C8 H8A 120.0 . .
C7 C8 H8A 120.0 . .
C10 C9 C8 120.9(3) . .
C10 C9 H9A 119.5 . .
C8 C9 H9A 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 Cl1 2.2720(8) .
Zn1 Cl1 2.2720(8) 2_656
Zn1 Cl3 2.2885(9) .
Zn1 Cl3 2.2885(9) 2_656
P2 C23 1.782(3) .
P2 C17 1.790(3) .
P2 C5 1.794(3) .
P2 C11 1.805(3) .
C17 C16 1.381(4) .
C17 C18 1.389(4) .
C22 C19 1.379(4) .
C22 C23 1.385(4) .
C22 H22A 0.9300 .
C23 C24 1.392(4) .
C18 C13 1.373(4) .
C18 H18A 0.9300 .
C16 C15 1.381(4) .
C16 H16A 0.9300 .
C5 C6 1.387(4) .
C5 C4 1.388(4) .
C11 C7 1.378(4) .
C11 C12 1.380(4) .
C15 C14 1.368(4) .
C15 H15A 0.9300 .
C10 C9 1.351(6) .
C10 C12 1.382(5) .
C10 H10A 0.9300 .
C13 C14 1.365(4) .
C13 H13A 0.9300 .
C19 C21 1.374(5) .
C19 H19A 0.9300 .
C6 C1 1.374(4) .
C6 H6A 0.9300 .
C24 C20 1.367(5) .
C24 H24A 0.9300 .
C20 C21 1.358(5) .
C20 H20A 0.9300 .
C14 H14A 0.9300 .
C12 H12A 0.9300 .
C4 C3 1.377(5) .
C4 H4A 0.9300 .
C21 H21A 0.9300 .
C3 C2 1.368(5) .
C3 H3A 0.9300 .
C2 C1 1.370(5) .
C2 H2A 0.9300 .
C7 C8 1.385(5) .
C7 H7A 0.9300 .
C1 H1A 0.9300 .
C8 C9 1.368(6) .
C8 H8A 0.9300 .
C9 H9A 0.9300 .
