#------------------------------------------------------------------------------
#$Date: 2016-03-21 15:08:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178738 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/49/4084978.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_4084978
loop_
_publ_author_name
'Hupf, Emanuel'
'Lork, Enno'
'Mebs, Stefan'
'Chęcińska, Lilianna'
'Beckmann, Jens'
_publ_section_title
;
 Probing Donor--Acceptor Interactions inperi-Substituted
 Diphenylphosphinoacenaphthyl--Element Dichlorides of Group 13 and 15
 Elements
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7247
_journal_paper_doi               10.1021/om501036c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C24 H18 Cl2 Ga P'
_chemical_formula_weight         477.97
_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                99.31(2)
_cell_angle_beta                 97.45(2)
_cell_angle_gamma                111.18(2)
_cell_formula_units_Z            2
_cell_length_a                   8.585(2)
_cell_length_b                   9.585(2)
_cell_length_c                   14.360(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.818
_cell_measurement_theta_min      5.494
_cell_volume                     1064.3(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGX
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3711
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.71
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.098
_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     253
_refine_ls_number_reflns         3711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0696P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                2807
_reflns_number_total             3711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501036c_si_003.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4084974--4084984.cif.'
_cod_original_cell_volume        1064.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084978
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ga1 Ga 0.45444(7) 0.21399(6) 0.74187(4) 0.02534(17) Uani 1 1 d .
P1 P 0.24167(15) 0.28235(13) 0.80900(8) 0.0235(3) Uani 1 1 d .
Cl1 Cl 0.59896(16) 0.16657(15) 0.86125(9) 0.0368(3) Uani 1 1 d .
Cl2 Cl 0.62861(16) 0.39434(15) 0.68691(9) 0.0408(3) Uani 1 1 d .
C19 C 0.1056(6) 0.0231(5) 0.6608(3) 0.0229(10) Uani 1 1 d .
C17 C -0.1032(6) 0.0813(5) 0.7420(3) 0.0271(10) Uani 1 1 d .
H17 H -0.1277 0.1446 0.7890 0.033 Uiso 1 1 calc R
C14 C -0.0320(6) -0.1067(5) 0.6037(3) 0.0260(10) Uani 1 1 d .
C10 C 0.2734(6) 0.0432(5) 0.6456(3) 0.0258(10) Uani 1 1 d .
C13 C -0.0140(6) -0.2138(5) 0.5313(3) 0.0301(11) Uani 1 1 d .
C15 C -0.2024(6) -0.1443(5) 0.6143(3) 0.0283(10) Uani 1 1 d .
C30 C 0.2286(6) 0.4602(5) 0.7906(3) 0.0250(10) Uani 1 1 d .
C35 C 0.0851(6) 0.4658(5) 0.7385(3) 0.0289(11) Uani 1 1 d .
H35 H -0.0097 0.3757 0.7105 0.035 Uiso 1 1 calc R
C16 C -0.2369(6) -0.0504(5) 0.6835(3) 0.0316(11) Uani 1 1 d .
H16 H -0.3483 -0.0734 0.6920 0.038 Uiso 1 1 calc R
C18 C 0.0646(6) 0.1193(5) 0.7313(3) 0.0243(10) Uani 1 1 d .
C20 C 0.2159(6) 0.2717(5) 0.9318(3) 0.0247(10) Uani 1 1 d .
C34 C 0.0830(7) 0.6065(6) 0.7281(4) 0.0362(12) Uani 1 1 d .
H34 H -0.0130 0.6107 0.6924 0.043 Uiso 1 1 calc R
C12 C 0.1456(7) -0.1918(6) 0.5151(3) 0.0359(12) Uani 1 1 d .
H12 H 0.1611 -0.2598 0.4668 0.043 Uiso 1 1 calc R
C11 C 0.2878(7) -0.0630(5) 0.5735(3) 0.0320(11) Uani 1 1 d .
H11 H 0.3961 -0.0497 0.5624 0.038 Uiso 1 1 calc R
C31 C 0.3704(7) 0.5953(5) 0.8322(4) 0.0437(14) Uani 1 1 d .
H31 H 0.4681 0.5917 0.8664 0.052 Uiso 1 1 calc R
C23 C 0.1566(7) 0.2362(6) 1.1125(4) 0.0403(13) Uani 1 1 d .
H23 H 0.1355 0.2242 1.1732 0.048 Uiso 1 1 calc R
C2 C -0.3127(7) -0.2930(6) 0.5439(4) 0.0385(13) Uani 1 1 d .
H2A H -0.3995 -0.2794 0.5002 0.046 Uiso 1 1 calc R
H2B H -0.3683 -0.3714 0.5775 0.046 Uiso 1 1 calc R
C21 C 0.2269(6) 0.1472(5) 0.9651(3) 0.0312(11) Uani 1 1 d .
H21 H 0.2541 0.0750 0.9265 0.037 Uiso 1 1 calc R
C33 C 0.2216(7) 0.7389(6) 0.7702(4) 0.0423(13) Uani 1 1 d .
H33 H 0.2190 0.8330 0.7634 0.051 Uiso 1 1 calc R
C22 C 0.1974(6) 0.1303(6) 1.0560(4) 0.0355(12) Uani 1 1 d .
H22 H 0.2053 0.0471 1.0787 0.043 Uiso 1 1 calc R
C24 C 0.1468(8) 0.3608(7) 1.0793(4) 0.0475(14) Uani 1 1 d .
H24 H 0.1210 0.4334 1.1184 0.057 Uiso 1 1 calc R
C32 C 0.3651(7) 0.7341(6) 0.8225(5) 0.0540(16) Uani 1 1 d .
H32 H 0.4587 0.8249 0.8512 0.065 Uiso 1 1 calc R
C25 C 0.1748(7) 0.3783(6) 0.9894(3) 0.0383(12) Uani 1 1 d .
H25 H 0.1661 0.4616 0.9671 0.046 Uiso 1 1 calc R
C1 C -0.1881(7) -0.3382(6) 0.4882(4) 0.0419(13) Uani 1 1 d .
H1A H -0.1902 -0.4373 0.4963 0.050 Uiso 1 1 calc R
H1B H -0.2191 -0.3432 0.4200 0.050 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C10 Ga1 Cl2 116.68(13)
C10 Ga1 Cl1 119.97(13)
Cl2 Ga1 Cl1 109.08(6)
C10 Ga1 P1 90.12(14)
Cl2 Ga1 P1 114.01(5)
Cl1 Ga1 P1 104.99(5)
C30 P1 C18 110.6(2)
C30 P1 C20 106.9(2)
C18 P1 C20 106.0(2)
C30 P1 Ga1 116.34(16)
C18 P1 Ga1 93.85(15)
C20 P1 Ga1 121.56(15)
C14 C19 C18 116.2(4)
C14 C19 C10 117.6(4)
C18 C19 C10 126.2(4)
C18 C17 C16 121.7(4)
C19 C14 C13 123.6(5)
C19 C14 C15 123.4(4)
C13 C14 C15 113.0(4)
C11 C10 C19 117.8(4)
C11 C10 Ga1 129.2(4)
C19 C10 Ga1 112.8(3)
C12 C13 C14 118.7(4)
C12 C13 C1 133.3(5)
C14 C13 C1 108.0(4)
C16 C15 C14 118.8(4)
C16 C15 C2 132.7(5)
C14 C15 C2 108.5(4)
C35 C30 C31 120.0(4)
C35 C30 P1 122.6(3)
C31 C30 P1 117.3(3)
C30 C35 C34 119.6(5)
C15 C16 C17 119.7(5)
C17 C18 C19 120.2(4)
C17 C18 P1 123.0(3)
C19 C18 P1 116.7(3)
C21 C20 C25 119.8(4)
C21 C20 P1 118.3(3)
C25 C20 P1 121.8(3)
C33 C34 C35 120.2(5)
C13 C12 C11 118.9(5)
C10 C11 C12 123.5(5)
C32 C31 C30 119.5(5)
C22 C23 C24 120.0(5)
C15 C2 C1 104.9(4)
C20 C21 C22 119.8(4)
C34 C33 C32 120.5(5)
C23 C22 C21 120.0(5)
C25 C24 C23 120.5(5)
C31 C32 C33 120.1(5)
C24 C25 C20 119.9(5)
C13 C1 C2 105.6(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ga1 C10 1.969(5)
Ga1 Cl2 2.1741(15)
Ga1 Cl1 2.1892(13)
Ga1 P1 2.4108(14)
P1 C30 1.807(4)
P1 C18 1.811(5)
P1 C20 1.819(4)
C19 C14 1.405(6)
C19 C18 1.422(6)
C19 C10 1.433(6)
C17 C18 1.388(6)
C17 C16 1.406(6)
C14 C13 1.404(6)
C14 C15 1.409(7)
C10 C11 1.381(6)
C13 C12 1.365(7)
C13 C1 1.508(7)
C15 C16 1.366(7)
C15 C2 1.504(6)
C30 C35 1.378(6)
C30 C31 1.392(7)
C35 C34 1.387(6)
C20 C21 1.384(6)
C20 C25 1.385(6)
C34 C33 1.366(7)
C12 C11 1.424(7)
C31 C32 1.377(7)
C23 C22 1.369(7)
C23 C24 1.381(7)
C2 C1 1.554(8)
C21 C22 1.386(7)
C33 C32 1.377(8)
C24 C25 1.368(7)
