#------------------------------------------------------------------------------
#$Date: 2019-11-28 14:29:22 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243948 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/54/7125481.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_7125481
loop_
_publ_author_name
'Brask, J. K.'
'Fickes, M. G.'
'Sangtrirutnugul, P.'
'Durà-Vilà, V'
'Odom, A. L.'
'Cummins, C. C.'
_publ_section_title
;
 Niobium and vanadium iminophosphinimide complexes.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1676
_journal_page_last               1677
_journal_paper_doi               10.1039/b105584b
_journal_year                    2001
_chemical_formula_sum            'C40 H63 N5 Nb P'
_chemical_formula_weight         737.83
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                106.92(4)
_cell_angle_beta                 90.52(6)
_cell_angle_gamma                114.37(4)
_cell_formula_units_Z            2
_cell_length_a                   10.584(7)
_cell_length_b                   12.626(10)
_cell_length_c                   17.968(13)
_cell_measurement_temperature    183(2)
_cell_volume                     2069(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0932
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6162
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  0.9429
_exptl_absorpt_correction_T_min  0.7070
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.161
_refine_ls_goodness_of_fit_obs   1.211
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.337
_refine_ls_restrained_S_obs      1.211
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_obs          0.0736
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+13.1256P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1678
_refine_ls_wR_factor_obs         0.1301
_reflns_number_observed          2885
_reflns_number_total             3802
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b105584b.txt
_cod_data_source_block           f
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.1256P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.1256P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2069.4(26)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7125481
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Nb Nb 0.61670(10) -0.01208(9) 0.27089(5) 0.0220(4) Uani 1 d .
P P 0.4595(3) 0.0260(2) 0.44022(15) 0.0267(7) Uani 1 d .
N1 N 0.8038(8) -0.0091(7) 0.2948(4) 0.027(2) Uani 1 d .
N2 N 0.4890(8) -0.1746(7) 0.1865(4) 0.024(2) Uani 1 d .
N3 N 0.6317(8) 0.1342(7) 0.2388(4) 0.024(2) Uani 1 d .
N4 N 0.5469(8) 0.0001(7) 0.3617(4) 0.023(2) Uani 1 d .
N5 N 0.4140(8) -0.0947(7) 0.4777(4) 0.024(2) Uani 1 d .
C11 C 0.9011(10) 0.0349(9) 0.2429(6) 0.028(3) Uani 1 d .
C12 C 0.9806(10) 0.1592(10) 0.2585(6) 0.031(3) Uani 1 d .
H12A H 0.9654(10) 0.2149(10) 0.3017(6) 0.037 Uiso 1 calc R
C13 C 1.0831(11) 0.2068(10) 0.2130(6) 0.038(3) Uani 1 d .
C14 C 1.0983(11) 0.1218(12) 0.1487(7) 0.045(3) Uani 1 d .
H14A H 1.1648(11) 0.1510(12) 0.1158(7) 0.054 Uiso 1 calc R
C15 C 1.0207(11) -0.0024(11) 0.1312(6) 0.035(3) Uani 1 d .
C16 C 0.9222(11) -0.0458(10) 0.1786(6) 0.035(3) Uani 1 d .
H16A H 0.8686(11) -0.1318(10) 0.1669(6) 0.042 Uiso 1 calc R
C17 C 0.8741(11) -0.0232(10) 0.3635(6) 0.037(3) Uani 1 d .
C18 C 0.9738(12) -0.0801(11) 0.3369(6) 0.060(4) Uani 1 d .
H18A H 1.0466(12) -0.0279(11) 0.3132(6) 0.090 Uiso 1 calc R
H18B H 0.9217(12) -0.1618(11) 0.2981(6) 0.090 Uiso 1 calc R
H18C H 1.0175(12) -0.0875(11) 0.3823(6) 0.090 Uiso 1 calc R
C19 C 0.9564(12) 0.1038(10) 0.4250(6) 0.051(3) Uani 1 d .
H19A H 0.8927(12) 0.1414(10) 0.4425(6) 0.076 Uiso 1 calc R
H19B H 1.0300(12) 0.1561(10) 0.4017(6) 0.076 Uiso 1 calc R
H19C H 0.9993(12) 0.0951(10) 0.4701(6) 0.076 Uiso 1 calc R
C21 C 0.5515(10) -0.2557(9) 0.1524(5) 0.025(3) Uani 1 d .
C22 C 0.5879(11) -0.2704(9) 0.0761(6) 0.033(3) Uani 1 d .
H22A H 0.5676(11) -0.2285(9) 0.0450(6) 0.040 Uiso 1 calc R
C23 C 0.6531(11) -0.3456(10) 0.0461(6) 0.039(3) Uani 1 d .
C24 C 0.6822(12) -0.4062(10) 0.0910(8) 0.051(3) Uani 1 d .
H24A H 0.7249(12) -0.4591(10) 0.0695(8) 0.062 Uiso 1 calc R
C25 C 0.6506(13) -0.3922(10) 0.1670(7) 0.047(3) Uani 1 d .
C26 C 0.5827(11) -0.3184(9) 0.1959(6) 0.038(3) Uani 1 d .
H26A H 0.5570(11) -0.3107(9) 0.2470(6) 0.045 Uiso 1 calc R
C27 C 0.3343(11) -0.2261(9) 0.1599(6) 0.030(3) Uani 1 d .
C28 C 0.2985(11) -0.2554(10) 0.0708(5) 0.044(3) Uani 1 d .
H28A H 0.3304(11) -0.3164(10) 0.0421(5) 0.066 Uiso 1 calc R
H28B H 0.3456(11) -0.1801(10) 0.0570(5) 0.066 Uiso 1 calc R
H28C H 0.1968(11) -0.2882(10) 0.0566(5) 0.066 Uiso 1 calc R
C29 C 0.2523(11) -0.3457(8) 0.1793(6) 0.036(3) Uani 1 d .
H29A H 0.2845(11) -0.4074(8) 0.1522(6) 0.054 Uiso 1 calc R
H29B H 0.1519(11) -0.3768(8) 0.1618(6) 0.054 Uiso 1 calc R
H29C H 0.2686(11) -0.3289(8) 0.2362(6) 0.054 Uiso 1 calc R
C31 C 0.6183(10) 0.2364(9) 0.2961(5) 0.021(2) Uani 1 d .
C32 C 0.7325(10) 0.3489(9) 0.3320(5) 0.024(3) Uani 1 d .
H32A H 0.8235(10) 0.3586(9) 0.3210(5) 0.028 Uiso 1 calc R
C33 C 0.7177(11) 0.4480(9) 0.3836(6) 0.031(3) Uani 1 d .
C34 C 0.5843(12) 0.4296(10) 0.3990(6) 0.034(3) Uani 1 d .
H34A H 0.5716(12) 0.4973(10) 0.4321(6) 0.041 Uiso 1 calc R
C35 C 0.4667(11) 0.3166(11) 0.3686(6) 0.034(3) Uani 1 d .
C36 C 0.4859(11) 0.2206(9) 0.3153(5) 0.024(3) Uani 1 d .
H36A H 0.4075(11) 0.1435(9) 0.2919(5) 0.029 Uiso 1 calc R
C37 C 0.6481(11) 0.1512(9) 0.1591(5) 0.031(3) Uani 1 d .
C38 C 0.6615(12) 0.0418(9) 0.1036(5) 0.043(3) Uani 1 d .
H38A H 0.5790(12) -0.0337(9) 0.1011(5) 0.064 Uiso 1 calc R
H38B H 0.7461(12) 0.0382(9) 0.1227(5) 0.064 Uiso 1 calc R
H38C H 0.6680(12) 0.0501(9) 0.0510(5) 0.064 Uiso 1 calc R
C39 C 0.5148(11) 0.1575(10) 0.1274(6) 0.045(3) Uani 1 d .
H39A H 0.5054(11) 0.2282(10) 0.1631(6) 0.068 Uiso 1 calc R
H39B H 0.4317(11) 0.0819(10) 0.1240(6) 0.068 Uiso 1 calc R
H39C H 0.5233(11) 0.1663(10) 0.0750(6) 0.068 Uiso 1 calc R
C48 C 0.2831(11) -0.1310(9) 0.2026(6) 0.038(3) Uani 1 d .
H48A H 0.3046(11) -0.1109(9) 0.2595(6) 0.058 Uiso 1 calc R
H48B H 0.1815(11) -0.1646(9) 0.1875(6) 0.058 Uiso 1 calc R
H48C H 0.3303(11) -0.0564(9) 0.1881(6) 0.058 Uiso 1 calc R
C51 C 0.3224(9) -0.2268(8) 0.4387(5) 0.022(2) Uani 1 d .
C52 C 0.4045(10) -0.2880(9) 0.3891(6) 0.041(3) Uani 1 d .
H52A H 0.4838(10) -0.2791(9) 0.4229(6) 0.062 Uiso 1 calc R
H52B H 0.4395(10) -0.2488(9) 0.3490(6) 0.062 Uiso 1 calc R
H52C H 0.3431(10) -0.3754(9) 0.3633(6) 0.062 Uiso 1 calc R
C53 C 0.2726(11) -0.2883(9) 0.5012(6) 0.041(3) Uani 1 d .
H53A H 0.3539(11) -0.2784(9) 0.5339(6) 0.062 Uiso 1 calc R
H53B H 0.2121(11) -0.3760(9) 0.4757(6) 0.062 Uiso 1 calc R
H53C H 0.2198(11) -0.2500(9) 0.5343(6) 0.062 Uiso 1 calc R
C54 C 0.1993(11) -0.2402(9) 0.3868(6) 0.040(3) Uani 1 d .
H54A H 0.1468(11) -0.2007(9) 0.4191(6) 0.061 Uiso 1 calc R
H54B H 0.1377(11) -0.3276(9) 0.3611(6) 0.061 Uiso 1 calc R
H54C H 0.2338(11) -0.2010(9) 0.3468(6) 0.061 Uiso 1 calc R
C58 C 0.7628(11) -0.1058(10) 0.3999(6) 0.048(3) Uani 1 d .
H58A H 0.6972(11) -0.0704(10) 0.4175(6) 0.072 Uiso 1 calc R
H58B H 0.8076(11) -0.1129(10) 0.4450(6) 0.072 Uiso 1 calc R
H58C H 0.7118(11) -0.1874(10) 0.3608(6) 0.072 Uiso 1 calc R
C131 C 1.1693(13) 0.3440(10) 0.2305(7) 0.064(4) Uani 1 d .
H13A H 1.1442(13) 0.3888(10) 0.2777(7) 0.096 Uiso 1 calc R
H13B H 1.1500(13) 0.3676(10) 0.1858(7) 0.096 Uiso 1 calc R
H13C H 1.2692(13) 0.3641(10) 0.2391(7) 0.096 Uiso 1 calc R
C151 C 1.0422(12) -0.0935(11) 0.0614(6) 0.054(3) Uani 1 d .
H15A H 0.9778(12) -0.1775(11) 0.0582(6) 0.081 Uiso 1 calc R
H15B H 1.1391(12) -0.0828(11) 0.0683(6) 0.081 Uiso 1 calc R
H15C H 1.0234(12) -0.0786(11) 0.0128(6) 0.081 Uiso 1 calc R
C231 C 0.6856(12) -0.3668(10) -0.0375(6) 0.056(4) Uani 1 d .
H23A H 0.6588(12) -0.3169(10) -0.0613(6) 0.084 Uiso 1 calc R
H23B H 0.6326(12) -0.4539(10) -0.0682(6) 0.084 Uiso 1 calc R
H23C H 0.7862(12) -0.3433(10) -0.0371(6) 0.084 Uiso 1 calc R
C251 C 0.6801(15) -0.4587(11) 0.2184(7) 0.077(4) Uani 1 d .
H25A H 0.6496(15) -0.4355(11) 0.2696(7) 0.115 Uiso 1 calc R
H25B H 0.7809(15) -0.4359(11) 0.2261(7) 0.115 Uiso 1 calc R
H25C H 0.6287(15) -0.5477(11) 0.1927(7) 0.115 Uiso 1 calc R
C310 C 0.7794(11) 0.2665(9) 0.1608(6) 0.040(3) Uani 1 d .
H31A H 0.7741(11) 0.3394(9) 0.1964(6) 0.061 Uiso 1 calc R
H31B H 0.7848(11) 0.2728(9) 0.1077(6) 0.061 Uiso 1 calc R
H31C H 0.8630(11) 0.2610(9) 0.1794(6) 0.061 Uiso 1 calc R
C331 C 0.8418(11) 0.5684(9) 0.4213(6) 0.050(3) Uani 1 d .
H33A H 0.9267(11) 0.5632(9) 0.4030(6) 0.075 Uiso 1 calc R
H33B H 0.8510(11) 0.5879(9) 0.4786(6) 0.075 Uiso 1 calc R
H33C H 0.8291(11) 0.6329(9) 0.4070(6) 0.075 Uiso 1 calc R
C351 C 0.3251(11) 0.2957(10) 0.3943(6) 0.052(3) Uani 1 d .
H35A H 0.2569(11) 0.2110(10) 0.3664(6) 0.079 Uiso 1 calc R
H35B H 0.2942(11) 0.3528(10) 0.3822(6) 0.079 Uiso 1 calc R
H35C H 0.3325(11) 0.3097(10) 0.4511(6) 0.079 Uiso 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'
Nb Nb -2.0727 0.6215 '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
N4 Nb N1 105.1(3) . .
N4 Nb N3 107.2(3) . .
N1 Nb N3 112.9(3) . .
N4 Nb N2 110.4(3) . .
N1 Nb N2 110.0(3) . .
N3 Nb N2 111.0(3) . .
N4 P N5 105.1(4) . 2_656
N4 P N5 108.7(4) . .
N5 P N5 79.9(4) 2_656 .
N4 P P 112.2(3) . 2_656
N5 P P 40.1(2) 2_656 2_656
N5 P P 39.8(2) . 2_656
C11 N1 C17 112.1(7) . .
C11 N1 Nb 113.2(6) . .
C17 N1 Nb 133.7(6) . .
C21 N2 C27 114.8(7) . .
C21 N2 Nb 116.4(6) . .
C27 N2 Nb 128.6(6) . .
C31 N3 C37 112.2(7) . .
C31 N3 Nb 119.3(5) . .
C37 N3 Nb 128.4(5) . .
P N4 Nb 167.0(5) . .
C51 N5 P 128.7(6) . 2_656
C51 N5 P 129.0(6) . .
P N5 P 100.1(4) 2_656 .
C12 C11 C16 118.3(10) . .
C12 C11 N1 120.2(9) . .
C16 C11 N1 121.5(9) . .
C11 C12 C13 122.6(10) . .
C14 C13 C12 116.6(10) . .
C14 C13 C131 121.3(10) . .
C12 C13 C131 122.1(10) . .
C15 C14 C13 122.4(10) . .
C14 C15 C16 119.2(10) . .
C14 C15 C151 121.2(10) . .
C16 C15 C151 119.6(10) . .
C11 C16 C15 120.9(10) . .
C18 C17 C58 108.3(9) . .
C18 C17 N1 111.5(8) . .
C58 C17 N1 109.4(8) . .
C18 C17 C19 108.9(9) . .
C58 C17 C19 109.7(8) . .
N1 C17 C19 109.0(8) . .
C26 C21 C22 118.1(10) . .
C26 C21 N2 120.0(9) . .
C22 C21 N2 121.9(9) . .
C23 C22 C21 120.4(10) . .
C24 C23 C22 119.8(10) . .
C24 C23 C231 119.7(11) . .
C22 C23 C231 120.5(11) . .
C23 C24 C25 121.6(10) . .
C24 C25 C26 118.1(10) . .
C24 C25 C251 123.1(11) . .
C26 C25 C251 118.7(11) . .
C21 C26 C25 122.0(10) . .
N2 C27 C48 108.5(8) . .
N2 C27 C28 112.7(8) . .
C48 C27 C28 108.0(8) . .
N2 C27 C29 111.2(8) . .
C48 C27 C29 108.8(8) . .
C28 C27 C29 107.5(8) . .
C32 C31 C36 118.9(9) . .
C32 C31 N3 122.4(8) . .
C36 C31 N3 118.7(8) . .
C31 C32 C33 122.0(9) . .
C34 C33 C32 117.2(9) . .
C34 C33 C331 121.7(9) . .
C32 C33 C331 121.1(10) . .
C33 C34 C35 123.5(9) . .
C34 C35 C36 117.3(9) . .
C34 C35 C351 122.0(9) . .
C36 C35 C351 120.7(10) . .
C31 C36 C35 121.0(9) . .
N3 C37 C38 108.8(7) . .
N3 C37 C310 113.0(8) . .
C38 C37 C310 107.3(8) . .
N3 C37 C39 108.8(8) . .
C38 C37 C39 109.0(9) . .
C310 C37 C39 109.8(8) . .
N5 C51 C54 109.0(8) . .
N5 C51 C52 110.0(7) . .
C54 C51 C52 109.9(8) . .
N5 C51 C53 109.1(7) . .
C54 C51 C53 111.0(8) . .
C52 C51 C53 107.9(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb N4 1.790(7) .
Nb N1 2.005(8) .
Nb N3 2.037(7) .
Nb N2 2.050(8) .
P N4 1.719(8) .
P N5 1.727(8) 2_656
P N5 1.734(7) .
P P 2.653(5) 2_656
N1 C11 1.445(12) .
N1 C17 1.526(12) .
N2 C21 1.436(11) .
N2 C27 1.503(12) .
N3 C31 1.459(11) .
N3 C37 1.510(11) .
N5 C51 1.479(11) .
N5 P 1.727(8) 2_656
C11 C12 1.378(13) .
C11 C16 1.388(13) .
C12 C13 1.403(13) .
C13 C14 1.390(14) .
C13 C131 1.518(14) .
C14 C15 1.370(14) .
C15 C16 1.389(13) .
C15 C151 1.526(14) .
C17 C18 1.515(14) .
C17 C58 1.517(13) .
C17 C19 1.532(14) .
C21 C26 1.385(13) .
C21 C22 1.408(13) .
C22 C23 1.386(14) .
C23 C24 1.37(2) .
C23 C231 1.516(14) .
C24 C25 1.387(15) .
C25 C26 1.390(14) .
C25 C251 1.524(15) .
C27 C48 1.527(13) .
C27 C28 1.540(13) .
C27 C29 1.545(13) .
C31 C32 1.389(12) .
C31 C36 1.393(12) .
C32 C33 1.392(13) .
C33 C34 1.377(13) .
C33 C331 1.494(13) .
C34 C35 1.397(14) .
C35 C36 1.399(13) .
C35 C351 1.512(14) .
C37 C38 1.511(12) .
C37 C310 1.535(13) .
C37 C39 1.558(14) .
C51 C54 1.516(13) .
C51 C52 1.521(13) .
C51 C53 1.525(12) .
