#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:48:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179816 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/12/7011270.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_7011270
loop_
_publ_author_name
'Rivard, Eric'
'McWilliams, Andrew R.'
'Lough, Alan J.'
'Manners, Ian'
_publ_section_title
;
 Synthesis and characterization of perhalogenated
 diazaphosphametalletidines containing transition metals from group 4
 and 5
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2173
_journal_paper_doi               10.1039/b109905c
_journal_year                    2002
_chemical_formula_sum            'C6 H18 Cl6 N2 Nb P Si2'
_chemical_formula_weight         510.98
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.679(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3280(9)
_cell_length_b                   8.7650(8)
_cell_length_c                   12.4990(12)
_cell_measurement_reflns_used    1766
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.55
_cell_volume                     988.56(16)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2001)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick 1999)'
_computing_publication_material  'SHELXTL V5.1 (Sheldrick 1999)'
_computing_structure_refinement  'SHELXTL V5.1 (Sheldrick 1999)'
_computing_structure_solution    'SHELXTL V5.1 (Sheldrick 1999)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2963
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_T_max  0.9097
_exptl_absorpt_correction_T_min  0.7187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(10)
_refine_ls_extinction_coef       0.0073(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2963
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0431
_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)+0.0866P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                2532
_reflns_number_total             2963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109905c.txt
_cod_data_source_block           k0108
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7011270
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
Nb1 Nb 0.38801(7) 0.33105(7) 0.27933(5) 0.0338(2) Uani 1 1 d . . .
Cl1 Cl 0.5030(2) 0.1559(2) 0.41184(17) 0.0447(5) Uani 1 1 d . . .
Cl2 Cl 0.4872(2) 0.2009(3) 0.14920(17) 0.0467(5) Uani 1 1 d . . .
Cl3 Cl 0.1603(2) 0.2321(3) 0.17994(17) 0.0480(5) Uani 1 1 d . . .
Cl4 Cl 0.2622(2) 0.4251(3) 0.40654(16) 0.0427(5) Uani 1 1 d . . .
Cl5 Cl 0.5331(2) 0.8041(2) 0.30891(17) 0.0462(5) Uani 1 1 d . . .
Cl6 Cl 0.6353(2) 0.6211(3) 0.12811(16) 0.0474(5) Uani 1 1 d . . .
P1 P 0.5218(2) 0.5969(2) 0.24291(16) 0.0348(5) Uani 1 1 d . . .
Si1 Si 0.2111(2) 0.6161(3) 0.08300(17) 0.0393(5) Uani 1 1 d . . .
Si2 Si 0.7743(2) 0.4309(3) 0.40504(18) 0.0382(5) Uani 1 1 d . . .
N1 N 0.3580(6) 0.5384(8) 0.1895(5) 0.0352(14) Uani 1 1 d . . .
N2 N 0.5863(6) 0.4651(7) 0.3305(5) 0.0367(15) Uani 1 1 d . . .
C1 C 0.0412(9) 0.6183(12) 0.1357(7) 0.053(2) Uani 1 1 d . . .
H1A H 0.0318 0.5205 0.1713 0.079 Uiso 1 1 calc R . .
H1B H -0.0460 0.6345 0.0739 0.079 Uiso 1 1 calc R . .
H1C H 0.0484 0.7010 0.1896 0.079 Uiso 1 1 calc R . .
C2 C 0.2617(10) 0.8158(12) 0.0529(7) 0.056(2) Uani 1 1 d . . .
H2A H 0.3498 0.8135 0.0237 0.084 Uiso 1 1 calc R . .
H2B H 0.2826 0.8761 0.1211 0.084 Uiso 1 1 calc R . .
H2C H 0.1790 0.8621 -0.0019 0.084 Uiso 1 1 calc R . .
C3 C 0.1944(9) 0.4951(11) -0.0407(7) 0.052(2) Uani 1 1 d . . .
H3A H 0.2865 0.5004 -0.0646 0.078 Uiso 1 1 calc R . .
H3B H 0.1118 0.5316 -0.1004 0.078 Uiso 1 1 calc R . .
H3C H 0.1759 0.3893 -0.0227 0.078 Uiso 1 1 calc R . .
C4 C 0.7876(9) 0.3834(11) 0.5513(6) 0.047(2) Uani 1 1 d . . .
H4A H 0.7447 0.2822 0.5557 0.070 Uiso 1 1 calc R . .
H4B H 0.7332 0.4595 0.5829 0.070 Uiso 1 1 calc R . .
H4C H 0.8919 0.3832 0.5929 0.070 Uiso 1 1 calc R . .
C5 C 0.8460(9) 0.2793(11) 0.3310(7) 0.053(2) Uani 1 1 d . . .
H5A H 0.8055 0.1807 0.3462 0.080 Uiso 1 1 calc R . .
H5B H 0.9543 0.2766 0.3562 0.080 Uiso 1 1 calc R . .
H5C H 0.8162 0.2997 0.2514 0.080 Uiso 1 1 calc R . .
C6 C 0.8795(9) 0.6130(11) 0.4031(7) 0.050(2) Uani 1 1 d . . .
H6A H 0.8307 0.6962 0.4326 0.075 Uiso 1 1 calc R . .
H6B H 0.8818 0.6368 0.3270 0.075 Uiso 1 1 calc R . .
H6C H 0.9811 0.6010 0.4488 0.075 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
Nb Nb -2.0727 0.6215 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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 Nb1 N2 71.1(2) . . ?
N1 Nb1 Cl1 157.58(17) . . ?
N2 Nb1 Cl1 86.66(17) . . ?
N1 Nb1 Cl3 93.25(17) . . ?
N2 Nb1 Cl3 163.53(17) . . ?
Cl1 Nb1 Cl3 109.15(8) . . ?
N1 Nb1 Cl4 92.08(17) . . ?
N2 Nb1 Cl4 98.42(17) . . ?
Cl1 Nb1 Cl4 88.22(8) . . ?
Cl3 Nb1 Cl4 86.99(7) . . ?
N1 Nb1 Cl2 94.10(17) . . ?
N2 Nb1 Cl2 90.65(17) . . ?
Cl1 Nb1 Cl2 88.91(8) . . ?
Cl3 Nb1 Cl2 85.21(7) . . ?
Cl4 Nb1 Cl2 170.30(8) . . ?
N1 Nb1 P1 35.41(17) . . ?
N2 Nb1 P1 35.77(17) . . ?
Cl1 Nb1 P1 122.43(7) . . ?
Cl3 Nb1 P1 128.23(7) . . ?
Cl4 Nb1 P1 98.09(7) . . ?
Cl2 Nb1 P1 91.26(7) . . ?
N1 P1 N2 102.1(3) . . ?
N1 P1 Cl5 114.4(3) . . ?
N2 P1 Cl5 113.9(3) . . ?
N1 P1 Cl6 111.1(2) . . ?
N2 P1 Cl6 113.1(2) . . ?
Cl5 P1 Cl6 102.64(13) . . ?
N1 P1 Nb1 50.6(2) . . ?
N2 P1 Nb1 51.6(2) . . ?
Cl5 P1 Nb1 133.50(11) . . ?
Cl6 P1 Nb1 123.85(11) . . ?
N1 Si1 C3 106.9(4) . . ?
N1 Si1 C1 107.5(3) . . ?
C3 Si1 C1 113.7(4) . . ?
N1 Si1 C2 108.7(4) . . ?
C3 Si1 C2 109.9(4) . . ?
C1 Si1 C2 110.0(5) . . ?
N2 Si2 C5 107.0(3) . . ?
N2 Si2 C4 111.3(3) . . ?
C5 Si2 C4 113.1(4) . . ?
N2 Si2 C6 107.3(3) . . ?
C5 Si2 C6 110.5(4) . . ?
C4 Si2 C6 107.5(4) . . ?
P1 N1 Si1 131.7(4) . . ?
P1 N1 Nb1 94.0(3) . . ?
Si1 N1 Nb1 134.1(3) . . ?
P1 N2 Si2 128.7(4) . . ?
P1 N2 Nb1 92.6(3) . . ?
Si2 N2 Nb1 136.0(4) . . ?
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
Nb1 N1 2.117(7) . ?
Nb1 N2 2.147(6) . ?
Nb1 Cl1 2.313(2) . ?
Nb1 Cl3 2.339(2) . ?
Nb1 Cl4 2.3516(19) . ?
Nb1 Cl2 2.359(2) . ?
Nb1 P1 2.735(2) . ?
Cl5 P1 1.987(3) . ?
Cl6 P1 1.999(3) . ?
P1 N1 1.589(6) . ?
P1 N2 1.601(6) . ?
Si1 N1 1.786(7) . ?
Si1 C3 1.849(9) . ?
Si1 C1 1.864(8) . ?
Si1 C2 1.875(10) . ?
Si2 N2 1.790(6) . ?
Si2 C5 1.839(9) . ?
Si2 C4 1.849(8) . ?
Si2 C6 1.877(9) . ?
