#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:29:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179143 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/04/4310434.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_4310434
loop_
_publ_author_name
'Eric Rivard'
'Alan J. Lough'
'Tristram Chivers'
'Ian Manners'
_publ_section_title
;
 Synthesis of Linear and Cyclic Carbophosphazenes via an Oxidative
 Chlorination Strategy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              802
_journal_page_last               811
_journal_paper_doi               10.1021/ic034954c
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C7 H5 Cl9 Ga N4 P3'
_chemical_formula_sum            'C7 H5 Cl9 Ga N4 P3'
_chemical_formula_weight         626.83
_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                103.6300(9)
_cell_angle_beta                 109.1460(10)
_cell_angle_gamma                91.4420(14)
_cell_formula_units_Z            2
_cell_length_a                   9.1460(2)
_cell_length_b                   10.0440(3)
_cell_length_c                   12.4390(4)
_cell_measurement_reflns_used    18709
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     1042.52(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.12'
_computing_publication_material  'SHELXTL V6.12'
_computing_structure_refinement  'SHELXTL V6.12(Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scan and ω scans with κ offsets'
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13106
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.704
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995) 
;
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0033(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0388
_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)+(0.0400P)²+0.0593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                3702
_reflns_number_total             4743
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic034954csi20031103_051734_6.cif
_cod_data_source_block           compound(10)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4310434
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.53112(4) -0.31816(4) 0.78422(3) 0.02354(12) Uani 1 1 d . . .
Cl1 Cl 0.48151(9) -0.26623(9) 0.46478(7) 0.0337(2) Uani 1 1 d . . .
Cl2 Cl 0.46521(9) -0.02240(9) 0.66763(7) 0.0319(2) Uani 1 1 d . . .
Cl3 Cl 0.29662(9) -0.34420(10) 0.65986(7) 0.0353(2) Uani 1 1 d . . .
Cl4 Cl 0.55606(10) -0.17353(10) 0.94841(8) 0.0420(2) Uani 1 1 d . . .
Cl5 Cl 0.60080(10) -0.51625(9) 0.80541(8) 0.0364(2) Uani 1 1 d . . .
Cl6 Cl 0.87382(9) -0.43102(9) 0.64314(8) 0.0351(2) Uani 1 1 d . . .
Cl7 Cl 1.21046(9) -0.40104(10) 0.91983(8) 0.0361(2) Uani 1 1 d . . .
Cl8 Cl 1.05582(10) -0.31252(10) 1.11360(7) 0.0379(2) Uani 1 1 d . . .
Cl9 Cl 1.20324(10) -0.08893(10) 1.03017(9) 0.0458(3) Uani 1 1 d . . .
P1 P 0.61066(9) -0.14532(9) 0.61931(7) 0.02376(19) Uani 1 1 d . . .
P2 P 0.85733(9) -0.25448(9) 0.75252(7) 0.02314(19) Uani 1 1 d . . .
P3 P 1.07649(9) -0.26957(9) 0.97302(7) 0.0253(2) Uani 1 1 d . . .
N1 N 0.6696(3) -0.2354(3) 0.7163(2) 0.0213(5) Uani 1 1 d . . .
N2 N 0.7437(3) -0.0572(3) 0.6040(2) 0.0298(6) Uani 1 1 d . . .
N3 N 0.9580(3) -0.1326(3) 0.7373(2) 0.0254(6) Uani 1 1 d . . .
N4 N 0.9141(3) -0.2744(3) 0.8824(2) 0.0262(6) Uani 1 1 d . . .
C1 C 0.8954(3) -0.0506(3) 0.6696(3) 0.0245(7) Uani 1 1 d . . .
C2 C 0.9991(3) 0.0629(3) 0.6652(3) 0.0242(7) Uani 1 1 d . . .
C3 C 0.9434(4) 0.1420(3) 0.5859(3) 0.0276(7) Uani 1 1 d . . .
H3A H 0.8396 0.1212 0.5319 0.033 Uiso 1 1 calc R . .
C4 C 1.0381(4) 0.2511(3) 0.5849(3) 0.0324(8) Uani 1 1 d . . .
H4A H 1.0002 0.3042 0.5297 0.039 Uiso 1 1 calc R . .
C5 C 1.1899(4) 0.2824(4) 0.6657(3) 0.0331(8) Uani 1 1 d . . .
H5A H 1.2553 0.3576 0.6660 0.040 Uiso 1 1 calc R . .
C6 C 1.2445(4) 0.2045(4) 0.7447(3) 0.0327(8) Uani 1 1 d . . .
H6A H 1.3474 0.2276 0.8001 0.039 Uiso 1 1 calc R . .
C7 C 1.1527(3) 0.0927(3) 0.7452(3) 0.0287(7) Uani 1 1 d . . .
H7A H 1.1927 0.0375 0.7983 0.034 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'
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'
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
_geom_angle_publ_flag
N1 Ga1 Cl4 105.91(7) . . ?
N1 Ga1 Cl5 109.00(8) . . ?
Cl4 Ga1 Cl5 112.88(4) . . ?
N1 Ga1 Cl3 107.19(7) . . ?
Cl4 Ga1 Cl3 112.03(4) . . ?
Cl5 Ga1 Cl3 109.57(4) . . ?
N2 P1 N1 115.23(14) . . ?
N2 P1 Cl1 109.61(11) . . ?
N1 P1 Cl1 110.37(10) . . ?
N2 P1 Cl2 109.55(12) . . ?
N1 P1 Cl2 107.23(10) . . ?
Cl1 P1 Cl2 104.25(5) . . ?
N4 P2 N3 113.55(14) . . ?
N4 P2 N1 107.16(13) . . ?
N3 P2 N1 113.29(14) . . ?
N4 P2 Cl6 107.87(11) . . ?
N3 P2 Cl6 108.28(11) . . ?
N1 P2 Cl6 106.34(10) . . ?
N4 P3 Cl8 109.40(11) . . ?
N4 P3 Cl7 115.17(11) . . ?
Cl8 P3 Cl7 106.20(6) . . ?
N4 P3 Cl9 114.97(12) . . ?
Cl8 P3 Cl9 105.50(6) . . ?
Cl7 P3 Cl9 104.81(5) . . ?
P1 N1 P2 113.41(15) . . ?
P1 N1 Ga1 124.24(13) . . ?
P2 N1 Ga1 122.34(15) . . ?
C1 N2 P1 122.9(3) . . ?
C1 N3 P2 122.6(2) . . ?
P3 N4 P2 132.46(18) . . ?
N3 C1 N2 126.5(3) . . ?
N3 C1 C2 118.2(3) . . ?
N2 C1 C2 115.3(3) . . ?
C3 C2 C7 120.2(3) . . ?
C3 C2 C1 120.5(3) . . ?
C7 C2 C1 119.3(3) . . ?
C4 C3 C2 120.5(3) . . ?
C3 C4 C5 119.5(3) . . ?
C6 C5 C4 120.0(3) . . ?
C5 C6 C7 121.4(3) . . ?
C6 C7 C2 118.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 N1 1.997(2) . ?
Ga1 Cl4 2.1478(9) . ?
Ga1 Cl5 2.1529(10) . ?
Ga1 Cl3 2.1602(8) . ?
Cl1 P1 1.9756(11) . ?
Cl2 P1 1.9780(11) . ?
Cl6 P2 2.0072(11) . ?
Cl7 P3 1.9708(11) . ?
Cl8 P3 1.9616(12) . ?
Cl9 P3 1.9715(12) . ?
P1 N2 1.573(3) . ?
P1 N1 1.637(3) . ?
P2 N4 1.589(3) . ?
P2 N3 1.596(3) . ?
P2 N1 1.654(2) . ?
P3 N4 1.534(3) . ?
N2 C1 1.350(4) . ?
N3 C1 1.323(4) . ?
C1 C2 1.487(4) . ?
C2 C3 1.386(5) . ?
C2 C7 1.405(4) . ?
C3 C4 1.384(5) . ?
C4 C5 1.396(5) . ?
C5 C6 1.374(5) . ?
C6 C7 1.388(5) . ?
