#------------------------------------------------------------------------------
#$Date: 2025-08-19 01:52:38 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301791 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/33/2003321.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003321
loop_
_publ_author_name
'Carson, C. C.'
'Pike, R. D.'
'Carpenter, G. B.'
_publ_section_title
;
 Azidotetrakis(trimethylphosphine)nickel(II) Tetrafluoroborate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              595
_journal_page_last               598
_journal_paper_doi               10.1107/S0108270194010553
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C12 H36 N3 Ni P4 1+, B F4 1-'
_chemical_formula_structural     'Ni N3 (P (C H3)3)4 B F4'
_chemical_formula_sum            'C12 H36 B F4 N3 Ni P4'
_chemical_formula_weight         491.84
_chemical_melting_point          408.15
_chemical_name_systematic
;
azidotetrakis(trimethylphosphine)nickel(II) tetrafluoroborate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.778(2)
_cell_length_b                   13.2816(13)
_cell_length_c                   26.188(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.15
_cell_volume                     4792.2(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1993)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL93 '
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL/PC (Siemens, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemans P4'
_diffrn_measurement_method       'Profile-fitted ω'
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.1088
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            5242
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .657
_refine_diff_density_min         -.633
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.852
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    'H atoms refined as riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4220
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      0.894
_refine_ls_restrained_S_obs      1.166
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_obs          0.0577
_refine_ls_shift/esd_max         -0.052
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.0743P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1529
_refine_ls_wR_factor_obs         0.1337
_reflns_number_observed          2018
_reflns_number_total             4220
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bk1077.cif
_cod_data_source_block           rp03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '135 C' was changed to '408.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4792.1(9)
_cod_database_code               2003321
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_occupancy
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 1 0.0554(1) 0.1954(1) 0.1057(1) 0.045(1) Uani d . . Ni
P1 1 -0.0521(1) 0.0847(2) 0.1435(1) 0.064(1) Uani d . . P
P2 1 0.0447(1) 0.2476(1) 0.0221(1) 0.054(1) Uani d . . P
P3 1 0.2006(1) 0.2210(1) 0.1483(1) 0.053(1) Uani d . . P
P4 1 -0.0137(1) 0.3283(1) 0.1353(1) 0.061(1) Uani d . . P
N1 1 0.1045(4) 0.0742(4) 0.0744(2) 0.064(2) Uani d . . N
N2 1 0.1775(5) 0.0430(5) 0.0588(2) 0.066(2) Uani d . . N
N3 1 0.2459(5) 0.0070(6) 0.0414(3) 0.135(3) Uani d . . N
C1 1 -0.1307(6) 0.1079(7) 0.1977(3) 0.104(3) Uani d . . C
H1A 1 -0.1721(26) 0.0507(17) 0.2029(12) 0.125 Uiso calc R . H
H1B 1 -0.1696(26) 0.1664(23) 0.1912(8) 0.125 Uiso calc R . H
H1C 1 -0.0919(6) 0.1188(37) 0.2276(5) 0.125 Uiso calc R . H
C2 1 0.0090(6) -0.0275(6) 0.1652(4) 0.117(3) Uani d . . C
H2A 1 -0.0382(7) -0.0761(17) 0.1761(19) 0.140 Uiso calc R . H
H2B 1 0.0509(29) -0.0110(10) 0.1933(13) 0.140 Uiso calc R . H
H2C 1 0.0469(32) -0.0551(23) 0.1378(7) 0.140 Uiso calc R . H
C3 1 -0.1370(5) 0.0334(7) 0.0972(3) 0.105(3) Uani d . . C
H3A 1 -0.1659(28) -0.0267(22) 0.1107(9) 0.126 Uiso calc R . H
H3B 1 -0.1031(9) 0.0176(37) 0.0662(8) 0.126 Uiso calc R . H
H3C 1 -0.1867(21) 0.0821(16) 0.0902(15) 0.126 Uiso calc R . H
C4 1 0.1597(5) 0.2487(7) -0.0110(2) 0.104(3) Uani d . . C
H4A 1 0.1487(5) 0.2572(39) -0.0469(3) 0.125 Uiso calc R . H
H4B 1 0.1928(17) 0.1862(16) -0.0051(16) 0.125 Uiso calc R . H
H4C 1 0.1986(15) 0.3033(23) 0.0015(14) 0.125 Uiso calc R . H
C5 1 -0.0031(7) 0.3651(6) -0.0028(3) 0.127(4) Uani d . . C
H5A 1 -0.0042(40) 0.3624(18) -0.0395(3) 0.152 Uiso calc R . H
H5B 1 0.0376(25) 0.4198(8) 0.0080(19) 0.152 Uiso calc R . H
H5C 1 -0.0677(17) 0.3753(22) 0.0098(18) 0.152 Uiso calc R . H
C6 1 -0.0250(6) 0.1607(6) -0.0140(3) 0.094(3) Uani d . . C
H6A 1 -0.0274(29) 0.1822(20) -0.0490(4) 0.113 Uiso calc R . H
H6B 1 -0.0897(11) 0.1577(26) -0.0005(11) 0.113 Uiso calc R . H
H6C 1 0.0043(19) 0.0953(10) -0.0121(15) 0.113 Uiso calc R . H
C7 1 0.2418(5) 0.1089(5) 0.1797(3) 0.087(2) Uani d . . C
H7A 1 0.3096(9) 0.1153(14) 0.1875(14) 0.105 Uiso calc R . H
H7B 1 0.2321(29) 0.0520(7) 0.1577(7) 0.105 Uiso calc R . H
H7C 1 0.2059(22) 0.0995(18) 0.2108(9) 0.105 Uiso calc R . H
C8 1 0.2271(6) 0.3115(5) 0.1980(3) 0.085(2) Uani d . . C
H8A 1 0.2939(10) 0.3053(22) 0.2080(12) 0.102 Uiso calc R . H
H8B 1 0.1861(22) 0.2989(21) 0.2269(7) 0.102 Uiso calc R . H
H8C 1 0.2154(30) 0.3783(6) 0.1854(6) 0.102 Uiso calc R . H
C9 1 0.2988(5) 0.2474(7) 0.1035(3) 0.094(3) Uani d . . C
H9A 1 0.3594(6) 0.2494(36) 0.1216(4) 0.113 Uiso calc R . H
H9B 1 0.2875(18) 0.3112(17) 0.0873(13) 0.113 Uiso calc R . H
H9C 1 0.3012(22) 0.1954(19) 0.0781(11) 0.113 Uiso calc R . H
C10 1 0.0457(5) 0.4435(5) 0.1184(3) 0.078(2) Uani d . . C
H10A 1 0.0245(23) 0.4963(8) 0.1408(10) 0.094 Uiso calc R . H
H10B 1 0.0298(23) 0.4607(16) 0.0838(6) 0.094 Uiso calc R . H
H10C 1 0.1147(5) 0.4352(10) 0.1215(15) 0.094 Uiso calc R . H
C11 1 -0.1383(5) 0.3483(7) 0.1138(3) 0.097(3) Uani d . . C
H11A 1 -0.1601(13) 0.4135(17) 0.1248(16) 0.116 Uiso calc R . H
H11B 1 -0.1795(8) 0.2973(23) 0.1281(15) 0.116 Uiso calc R . H
H11C 1 -0.1407(8) 0.3448(37) 0.0772(3) 0.116 Uiso calc R . H
C12 1 -0.0239(6) 0.3390(7) 0.2042(3) 0.098(3) Uani d . . C
H12A 1 -0.0390(34) 0.4074(10) 0.2132(3) 0.118 Uiso calc R . H
H12B 1 0.0365(13) 0.3200(35) 0.2198(3) 0.118 Uiso calc R . H
H12C 1 -0.0746(25) 0.2954(28) 0.2162(3) 0.118 Uiso calc R . H
B1A 0.50 0.5877(13) 0.1762(14) 0.1749(7) 0.091(3) Uiso d PD 1 B
F1A 0.50 0.6431(9) 0.2511(9) 0.1930(5) 0.125(5) Uiso d PD 1 F
F2A 0.50 0.6170(9) 0.0885(9) 0.1978(5) 0.143(4) Uiso d PD 1 F
F3A 0.50 0.5931(11) 0.1587(11) 0.1241(4) 0.164(5) Uiso d PD 1 F
F4A 0.50 0.4943(7) 0.1954(8) 0.1857(4) 0.122(4) Uiso d PD 1 F
B1B 0.50 0.5961(14) 0.1787(14) 0.1687(7) 0.091(3) Uiso d PD 2 B
F1B 0.50 0.6541(8) 0.2595(8) 0.1723(4) 0.104(4) Uiso d PD 2 F
F2B 0.50 0.6433(8) 0.1076(9) 0.1402(5) 0.134(4) Uiso d PD 2 F
F3B 0.50 0.5189(9) 0.2053(9) 0.1390(5) 0.141(4) Uiso d PD 2 F
F4B 0.50 0.5706(10) 0.1377(11) 0.2148(4) 0.161(5) Uiso d PD 2 F
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0033 .0016
H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000
B B 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0013 .0007
N N 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0061 .0033
F F 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0171 .0103
P P 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1023 .0942
Ni Ni 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .3393 1.11
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 P4 173.6(2) yes
N1 Ni1 P2 82.6(2) yes
P4 Ni1 P2 93.89(7) yes
N1 Ni1 P1 82.9(2) yes
P4 Ni1 P1 94.80(8) yes
P2 Ni1 P1 123.95(7) yes
N1 Ni1 P3 91.4(2) yes
P4 Ni1 P3 95.03(7) yes
P2 Ni1 P3 118.02(7) yes
P1 Ni1 P3 116.15(7) yes
C2 P1 C1 99.9(4) ?
C2 P1 C3 101.6(5) ?
C1 P1 C3 101.7(4) ?
C2 P1 Ni1 111.2(3) ?
C1 P1 Ni1 127.7(3) ?
C3 P1 Ni1 111.4(3) ?
C6 P2 C4 103.0(4) ?
C6 P2 C5 99.9(4) ?
C4 P2 C5 98.0(4) ?
C6 P2 Ni1 110.2(3) ?
C4 P2 Ni1 113.7(2) ?
C5 P2 Ni1 128.7(3) ?
C7 P3 C8 99.1(3) ?
C7 P3 C9 102.7(4) ?
C8 P3 C9 100.6(4) ?
C7 P3 Ni1 111.9(2) ?
C8 P3 Ni1 128.2(3) ?
C9 P3 Ni1 111.1(2) ?
C10 P4 C12 102.4(4) ?
C10 P4 C11 103.2(4) ?
C12 P4 C11 102.9(4) ?
C10 P4 Ni1 114.1(2) ?
C12 P4 Ni1 117.2(3) ?
C11 P4 Ni1 115.1(3) ?
N2 N1 Ni1 138.6(5) yes
N3 N2 N1 174.9(8) yes
F1A B1A F4A 109.2(14) ?
F1A B1A F3A 116.4(2) ?
F4A B1A F3A 107.1(14) ?
F1A B1A F2A 107.9(14) ?
F4A B1A F2A 110.5(14) ?
F3A B1A F2A 105.6(14) ?
F1B B1B F3B 107.2(13) ?
F1B B1B F4B 114.2(14) ?
F3B B1B F4B 114(2) ?
F1B B1B F2B 107.9(14) ?
F3B B1B F2B 103.8(13) ?
F4B B1B F2B 109.2(14) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 1.929(6) yes
Ni1 P4 2.152(2) yes
Ni1 P2 2.301(2) yes
Ni1 P1 2.309(2) yes
Ni1 P3 2.316(2) yes
P1 C2 1.804(8) yes
P1 C1 1.812(7) yes
P1 C3 1.817(7) yes
P2 C6 1.773(7) yes
P2 C4 1.806(7) yes
P2 C5 1.815(7) yes
P3 C7 1.793(7) yes
P3 C8 1.809(7) yes
P3 C9 1.825(6) yes
P4 C10 1.791(7) yes
P4 C12 1.815(7) yes
P4 C11 1.826(7) yes
N1 N2 1.162(7) yes
N2 N3 1.150(8) yes
B1A F1A 1.34(2) ?
B1A F4A 1.34(2) ?
B1A F3A 1.35(2) ?
B1A F2A 1.37(2) ?
B1B F1B 1.34(2) ?
B1B F3B 1.36(2) ?
B1B F4B 1.37(2) ?
B1B F2B 1.37(2) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 Ni1 P1 C2 43.2(4)
P4 Ni1 P1 C2 -142.9(4)
P2 Ni1 P1 C2 119.2(3)
P3 Ni1 P1 C2 -44.9(4)
N1 Ni1 P1 C1 165.4(4)
P4 Ni1 P1 C1 -20.7(4)
P2 Ni1 P1 C1 -118.6(4)
P3 Ni1 P1 C1 77.3(4)
N1 Ni1 P1 C3 -69.4(4)
P4 Ni1 P1 C3 104.6(3)
P2 Ni1 P1 C3 6.6(3)
P3 Ni1 P1 C3 -157.4(3)
N1 Ni1 P2 C6 55.0(4)
P4 Ni1 P2 C6 -119.7(3)
P1 Ni1 P2 C6 -21.2(3)
P3 Ni1 P2 C6 142.5(3)
N1 Ni1 P2 C4 -60.1(4)
P4 Ni1 P2 C4 125.3(4)
P1 Ni1 P2 C4 -136.3(3)
P3 Ni1 P2 C4 27.5(4)
N1 Ni1 P2 C5 176.9(5)
P4 Ni1 P2 C5 2.3(4)
P1 Ni1 P2 C5 100.7(4)
P3 Ni1 P2 C5 -95.5(4)
N1 Ni1 P3 C7 -48.2(3)
P4 Ni1 P3 C7 132.4(3)
P2 Ni1 P3 C7 -130.5(3)
P1 Ni1 P3 C7 34.5(3)
N1 Ni1 P3 C8 -170.4(3)
P4 Ni1 P3 C8 10.2(3)
P2 Ni1 P3 C8 107.3(3)
P1 Ni1 P3 C8 -87.7(3)
N1 Ni1 P3 C9 65.9(4)
P4 Ni1 P3 C9 -113.5(3)
P2 Ni1 P3 C9 -16.4(3)
P1 Ni1 P3 C9 148.6(3)
N1 Ni1 P4 C10 -113.4(16)
P2 Ni1 P4 C10 -57.3(3)
P1 Ni1 P4 C10 178.1(3)
P3 Ni1 P4 C10 61.3(3)
N1 Ni1 P4 C12 126.9(16)
P2 Ni1 P4 C12 -177.0(3)
P1 Ni1 P4 C12 58.4(3)
P3 Ni1 P4 C12 -58.4(3)
N1 Ni1 P4 C11 5.7(17)
P2 Ni1 P4 C11 61.8(3)
P1 Ni1 P4 C11 -62.8(3)
P3 Ni1 P4 C11 -179.6(3)
P4 Ni1 N1 N2 140.1(13)
P2 Ni1 N1 N2 83.5(8)
P1 Ni1 N1 N2 -150.8(8)
P3 Ni1 N1 N2 -34.6(8)
Ni1 N1 N2 N3 -161.(9)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168307580
