#------------------------------------------------------------------------------
#$Date: 2019-11-23 18:53:33 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 234732 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/20/7702075.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_7702075
loop_
_publ_author_name
'Benjamin, Sophie L.'
'Chang, Yao-Pang'
'Hector, Andrew L.'
'Jura, Marek'
'Levason, William'
'Reid, Gillian'
'Stenning, Gavin'
_publ_section_title
;
 Niobium tetrahalide complexes with neutral diphosphine ligands.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8192
_journal_page_last               8200
_journal_paper_doi               10.1039/c6dt01099g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C20 H32 Cl4 Nb P4'
_chemical_formula_sum            'C20 H32 Cl4 Nb P4'
_chemical_formula_weight         631.04
_chemical_name_common            '[NbCl4(o-DMPB)2]'
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9876(7)
_cell_length_b                   8.9876(7)
_cell_length_c                   16.1482(11)
_cell_measurement_reflns_used    2286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.1
_cell_volume                     1304.40(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2204
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.941
_diffrn_reflns_theta_min         4.081
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
; 
 Flack x determined using 263 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0158P)²+13.9926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.672
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                703
_reflns_number_total             754
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01099g2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' 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.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1304.4(2)
_cod_database_code               7702075
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_file
; 
  
    shelx.res created by SHELXL-2014/7 
  
  
TITL shelx in I-42m 
CELL 0.71073   8.9876   8.9876  16.1482  90.000  90.000  90.000 
ZERR    2.00   0.0007   0.0007   0.0011   0.000   0.000   0.000 
LATT -2 
SYMM -X, -Y, Z 
SYMM Y, -X, -Z 
SYMM -Y, X, -Z 
SYMM -X, Y, -Z 
SYMM X, -Y, -Z 
SYMM -Y, -X, Z 
SYMM Y, X, Z 
SFAC C  H  P  Cl Nb 
UNIT 40 64 8 8 2 
OMIT  -4.00  54.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.08 0.04 0.02 
TEMP -173 
WGHT    0.015800   13.992596 
FVAR       0.59736 
MOLE 1 
NB1   5    0.000000    1.000000    1.000000    10.12500    0.03974    0.03974 = 
         0.01878    0.00000    0.00000    0.00000 
CL1   4   -0.183638    0.816362    0.955766    10.50000    0.03888    0.03888 = 
         0.03567   -0.00313   -0.00313   -0.00137 
P1    3    0.124833    0.875167    0.864494    10.50000    0.01573    0.01573 = 
         0.01694   -0.00119    0.00119    0.00207 
C1    1    0.100690    0.674987    0.854516    11.00000    0.04802    0.02038 = 
         0.02397   -0.00140    0.00450    0.00513 
AFIX 137 
H1A   2   -0.005321    0.652012    0.848335    11.00000   -1.50000 
H1B   2    0.139445    0.625575    0.904129    11.00000   -1.50000 
H1C   2    0.154942    0.639542    0.805709    11.00000   -1.50000 
AFIX   0 
C2    1    0.054603    0.945397    0.765520    10.50000    0.01818    0.01818 = 
         0.01289   -0.00331    0.00331   -0.00791 
C3    1    0.109821    0.890179    0.689536    10.50000    0.02243    0.02243 = 
         0.01785   -0.00525    0.00525   -0.00388 
AFIX  43 
H3    2    0.184558    0.815442    0.688895    10.50000   -1.20000 
AFIX   0 
C4    1    0.053562    0.946438    0.615887    10.50000    0.03131    0.03131 = 
         0.01058   -0.00435    0.00435   -0.01783 
AFIX  43 
H4    2    0.090356    0.909644    0.564679    10.50000   -1.20000 
AFIX   0 
HKLF 4 
  
REM  shelx in I-42m 
REM R1 =  0.0477 for     703 Fo > 4sig(Fo)  and  0.0523 for all     754 data 
REM     43 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0180     14.0397 
  
REM Highest difference peak  1.380,  deepest hole -0.876,  1-sigma level  0.118 
Q1    1  -0.0443  1.0443  1.0226  10.50000  0.05    1.38 
Q2    1  -0.1222  0.8778  0.9758  10.50000  0.05    0.90 
Q3    1   0.1252  1.0580  1.0305  11.00000  0.05    0.47 
Q4    1   0.0000  1.0000  0.8505  10.25000  0.05    0.46 
Q5    1   0.1728  0.8272  0.8449  10.50000  0.05    0.42 
;
_shelx_res_checksum              38427
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Nb1 Nb 0.0000 1.0000 1.0000 0.0327(6) Uani 1 8 d S T P
Cl1 Cl -0.1836(2) 0.8164(2) 0.95577(16) 0.0378(7) Uani 1 2 d S T P
P1 P 0.12483(19) 0.87517(19) 0.86449(13) 0.0161(5) Uani 1 2 d S T P
C1 C 0.1007(9) 0.6750(8) 0.8545(4) 0.0308(17) Uani 1 1 d . . .
H1A H -0.0053 0.6520 0.8483 0.046 Uiso 1 1 calc R U .
H1B H 0.1394 0.6256 0.9041 0.046 Uiso 1 1 calc R U .
H1C H 0.1549 0.6395 0.8057 0.046 Uiso 1 1 calc R U .
C2 C 0.0546(7) 0.9454(7) 0.7655(5) 0.0164(17) Uani 1 2 d S T P
C3 C 0.1098(8) 0.8902(8) 0.6895(5) 0.0209(19) Uani 1 2 d S T P
H3 H 0.1846 0.8154 0.6889 0.025 Uiso 1 2 calc R U P
C4 C 0.0536(9) 0.9464(9) 0.6159(5) 0.024(2) Uani 1 2 d S T P
H4 H 0.0904 0.9096 0.5647 0.029 Uiso 1 2 calc R U P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.0397(8) 0.0397(8) 0.0188(9) 0.000 0.000 0.000
Cl1 0.0389(10) 0.0389(10) 0.0357(14) -0.0031(9) -0.0031(9) -0.0014(14)
P1 0.0157(7) 0.0157(7) 0.0169(11) -0.0012(6) 0.0012(6) 0.0021(10)
C1 0.048(5) 0.020(3) 0.024(3) -0.001(3) 0.005(3) 0.005(3)
C2 0.018(3) 0.018(3) 0.013(4) -0.003(3) 0.003(3) -0.008(4)
C3 0.022(3) 0.022(3) 0.018(4) -0.005(3) 0.005(3) -0.004(4)
C4 0.031(3) 0.031(3) 0.011(4) -0.004(3) 0.004(3) -0.018(4)
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'
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
Cl1 Nb1 Cl1 145.97(13) . 2_575
Cl1 Nb1 Cl1 94.91(4) . 4_667
Cl1 Nb1 Cl1 94.91(4) 2_575 4_667
Cl1 Nb1 Cl1 94.91(4) . 3_467
Cl1 Nb1 Cl1 94.91(4) 2_575 3_467
Cl1 Nb1 Cl1 145.97(13) 4_667 3_467
Cl1 Nb1 P1 142.96(8) . 4_667
Cl1 Nb1 P1 71.07(8) 2_575 4_667
Cl1 Nb1 P1 76.30(5) 4_667 4_667
Cl1 Nb1 P1 76.30(5) 3_467 4_667
Cl1 Nb1 P1 76.30(5) . 2_575
Cl1 Nb1 P1 76.30(5) 2_575 2_575
Cl1 Nb1 P1 142.96(8) 4_667 2_575
Cl1 Nb1 P1 71.07(8) 3_467 2_575
P1 Nb1 P1 130.95(6) 4_667 2_575
Cl1 Nb1 P1 71.07(8) . 3_467
Cl1 Nb1 P1 142.96(8) 2_575 3_467
Cl1 Nb1 P1 76.30(5) 4_667 3_467
Cl1 Nb1 P1 76.30(5) 3_467 3_467
P1 Nb1 P1 71.89(10) 4_667 3_467
P1 Nb1 P1 130.95(6) 2_575 3_467
Cl1 Nb1 P1 76.30(5) . .
Cl1 Nb1 P1 76.30(5) 2_575 .
Cl1 Nb1 P1 71.07(8) 4_667 .
Cl1 Nb1 P1 142.96(8) 3_467 .
P1 Nb1 P1 130.95(6) 4_667 .
P1 Nb1 P1 71.89(10) 2_575 .
P1 Nb1 P1 130.95(6) 3_467 .
C1 P1 C1 103.2(5) 7_665 .
C1 P1 C2 102.9(3) 7_665 .
C1 P1 C2 102.9(3) . .
C1 P1 Nb1 115.6(2) 7_665 .
C1 P1 Nb1 115.6(2) . .
C2 P1 Nb1 114.9(3) . .
P1 C1 H1A 109.5 . .
P1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
P1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C2 C2 C3 119.8(6) 2_575 .
C2 C2 P1 119.2(3) 2_575 .
C3 C2 P1 121.0(7) . .
C4 C3 C2 119.2(9) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C4 C4 C3 121.0(6) 2_575 .
C4 C4 H4 119.5 2_575 .
C3 C4 H4 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl1 2.441(3) .
Nb1 Cl1 2.441(3) 2_575
Nb1 Cl1 2.441(3) 4_667
Nb1 Cl1 2.441(3) 3_467
Nb1 P1 2.703(2) 4_667
Nb1 P1 2.703(2) 2_575
Nb1 P1 2.703(2) 3_467
Nb1 P1 2.703(2) .
P1 C1 1.819(8) 7_665
P1 C1 1.819(8) .
P1 C2 1.831(9) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C2 1.388(19) 2_575
C2 C3 1.414(12) .
C3 C4 1.388(13) .
C3 H3 0.9500 .
C4 C4 1.36(2) 2_575
C4 H4 0.9500 .
