#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/50/7005098.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_7005098
loop_
_publ_author_name
'Landry, Victoria K.'
'Pang, Keliang'
'Quan, Stephanie M.'
'Parkin, Gerard'
_publ_section_title
;
 Tetrahedral nickel nitrosyl complexes with tripodal [N3] and [Se3]
 donor ancillary ligands: structural and computational evidence that a
 linear nitrosyl is a trivalent ligand.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              820
_journal_page_last               824
_journal_paper_doi               10.1039/b616674a
_journal_year                    2007
_chemical_formula_sum            'C45 H47.5 B N7 Ni O P0.5 Se3'
_chemical_formula_weight         1024.29
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   14.5179(5)
_cell_length_b                   14.5179(5)
_cell_length_c                   73.730(5)
_cell_measurement_reflns_used    9289
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.74
_cell_volume                     13458.1(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -96
_diffrn_reflns_number            24431
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    2.927
_exptl_absorpt_correction_T_max  0.7584
_exptl_absorpt_correction_T_min  0.7584
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             6204
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0315
_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)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                2347
_reflns_number_total             3489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b616674a.txt
_cod_data_source_block           nips10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' 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_cell_volume        13458.0(12)
_cod_original_sg_symbol_H-M      R-3c
_cod_original_formula_sum        'C45 H47.50 B N7 Ni O P0.50 Se3'
_cod_database_code               7005098
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Ni Ni 0.3333 0.6667 0.015150(7) 0.03909(15) Uani 1 3 d S . .
Se Se 0.50894(2) 0.77442(2) 0.028974(3) 0.04031(9) Uani 1 1 d . . .
N1 N 0.3333 0.6667 -0.00700(5) 0.0466(10) Uani 1 3 d S . .
O1 O 0.3333 0.6667 -0.02268(5) 0.1104(18) Uani 1 3 d S . .
B B 0.3333 0.6667 0.06752(6) 0.0319(10) Uani 1 3 d S . .
H1 H 0.3333 0.6667 0.0852(5) 0.048 Uiso 1 3 d S . .
N11 N 0.42659(15) 0.64967(15) 0.06200(2) 0.0309(4) Uani 1 1 d . . .
N12 N 0.56767(15) 0.65190(15) 0.05121(2) 0.0344(4) Uani 1 1 d . . .
C11 C 0.49875(18) 0.68774(18) 0.04842(3) 0.0325(5) Uani 1 1 d . . .
C12 C 0.4500(2) 0.58632(19) 0.07299(3) 0.0383(6) Uani 1 1 d . . .
H12A H 0.4115 0.5490 0.0833 0.046 Uiso 1 1 calc R . .
C13 C 0.5363(2) 0.5872(2) 0.06643(3) 0.0403(6) Uani 1 1 d . . .
H13A H 0.5693 0.5509 0.0712 0.048 Uiso 1 1 calc R . .
C21 C 0.66094(18) 0.67509(19) 0.04079(3) 0.0355(6) Uani 1 1 d . . .
C22 C 0.6547(2) 0.5980(2) 0.02879(3) 0.0411(6) Uani 1 1 d . . .
C23 C 0.7481(2) 0.6188(2) 0.02010(3) 0.0462(6) Uani 1 1 d . . .
H23A H 0.7462 0.5678 0.0120 0.055 Uiso 1 1 calc R . .
C24 C 0.8431(2) 0.7112(3) 0.02282(4) 0.0505(7) Uani 1 1 d . . .
C25 C 0.8453(2) 0.7866(2) 0.03467(3) 0.0463(7) Uani 1 1 d . . .
H25A H 0.9096 0.8504 0.0365 0.056 Uiso 1 1 calc R . .
C26 C 0.7537(2) 0.7696(2) 0.04390(3) 0.0384(6) Uani 1 1 d . . .
C27 C 0.5520(2) 0.4979(2) 0.02521(4) 0.0614(8) Uani 1 1 d . . .
H27A H 0.4960 0.5149 0.0233 0.092 Uiso 1 1 calc R . .
H27B H 0.5343 0.4505 0.0355 0.092 Uiso 1 1 calc R . .
H27C H 0.5592 0.4635 0.0145 0.092 Uiso 1 1 calc R . .
C28 C 0.9430(2) 0.7305(3) 0.01303(4) 0.0766(10) Uani 1 1 d . . .
H28A H 0.9934 0.8062 0.0126 0.115 Uiso 1 1 calc R . .
H28B H 0.9251 0.7028 0.0008 0.115 Uiso 1 1 calc R . .
H28C H 0.9746 0.6947 0.0195 0.115 Uiso 1 1 calc R . .
C29 C 0.7575(2) 0.8534(2) 0.05642(4) 0.0520(7) Uani 1 1 d . . .
H29A H 0.7266 0.8214 0.0680 0.078 Uiso 1 1 calc R . .
H29B H 0.7177 0.8839 0.0511 0.078 Uiso 1 1 calc R . .
H29C H 0.8309 0.9088 0.0582 0.078 Uiso 1 1 calc R . .
P1 P 0.3333 0.6667 -0.06627(3) 0.0436(6) Uani 0.50 3 d SP . .
C31 C 0.2174(3) 0.5574(3) -0.07704(6) 0.0408(14) Uani 0.50 1 d PG A -1
C32 C 0.1681(4) 0.4662(4) -0.06642(7) 0.053(2) Uani 0.50 1 d PG A -1
H32A H 0.1960 0.4652 -0.0550 0.063 Uiso 0.50 1 calc PR A -1
C33 C 0.0773(6) 0.3765(4) -0.07271(12) 0.064(3) Uani 0.50 1 d PG A -1
H33A H 0.0439 0.3148 -0.0655 0.077 Uiso 0.50 1 calc PR A -1
C34 C 0.0359(6) 0.3779(5) -0.08964(12) 0.083(6) Uani 0.50 1 d PG A -1
H34A H -0.0255 0.3172 -0.0939 0.099 Uiso 0.50 1 calc PR A -1
C35 C 0.0853(4) 0.4691(5) -0.10027(8) 0.059(3) Uani 0.50 1 d PG A -1
H35A H 0.0573 0.4701 -0.1117 0.071 Uiso 0.50 1 calc PR A -1
C36 C 0.1760(3) 0.5589(4) -0.09397(6) 0.0492(15) Uani 0.50 1 d PG A -1
H36A H 0.2094 0.6205 -0.1012 0.059 Uiso 0.50 1 calc PR A -1
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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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 Ni Se 114.594(12) . 2_665 ?
N1 Ni Se 114.594(12) . . ?
Se Ni Se 103.897(14) 2_665 . ?
N1 Ni Se 114.594(12) . 3_565 ?
Se Ni Se 103.897(14) 2_665 3_565 ?
Se Ni Se 103.897(14) . 3_565 ?
C11 Se Ni 100.55(7) . . ?
O1 N1 Ni 180.0 . . ?
N11 B N11 113.33(14) 2_665 3_565 ?
N11 B N11 113.33(14) 2_665 . ?
N11 B N11 113.33(14) 3_565 . ?
C11 N11 C12 107.87(19) . . ?
C11 N11 B 133.7(2) . . ?
C12 N11 B 118.3(2) . . ?
C11 N12 C13 109.12(18) . . ?
C11 N12 C21 128.09(18) . . ?
C13 N12 C21 122.78(19) . . ?
N11 C11 N12 107.52(18) . . ?
N11 C11 Se 129.00(17) . . ?
N12 C11 Se 123.47(16) . . ?
C13 C12 N11 108.7(2) . . ?
C12 C13 N12 106.7(2) . . ?
C26 C21 C22 122.9(2) . . ?
C26 C21 N12 118.7(2) . . ?
C22 C21 N12 118.3(2) . . ?
C23 C22 C21 117.0(2) . . ?
C23 C22 C27 121.3(2) . . ?
C21 C22 C27 121.7(2) . . ?
C24 C23 C22 122.6(3) . . ?
C23 C24 C25 118.5(2) . . ?
C23 C24 C28 120.8(3) . . ?
C25 C24 C28 120.8(3) . . ?
C24 C25 C26 121.4(3) . . ?
C21 C26 C25 117.6(2) . . ?
C21 C26 C29 121.9(2) . . ?
C25 C26 C29 120.4(2) . . ?
C31 P1 C31 102.36(17) 3_565 . ?
C31 P1 C31 102.36(17) 3_565 2_665 ?
C31 P1 C31 102.36(17) . 2_665 ?
C31 P1 C36 23.3(3) 3_565 11_564 ?
C31 P1 C36 92.3(4) . 11_564 ?
C31 P1 C36 125.4(3) 2_665 11_564 ?
C31 P1 C36 125.4(2) 3_565 10_454 ?
C31 P1 C36 23.3(2) . 10_454 ?
C31 P1 C36 92.3(3) 2_665 10_454 ?
C36 P1 C36 115.0(2) 11_564 10_454 ?
C31 P1 C36 92.3(7) 3_565 12_554 ?
C31 P1 C36 125.4(4) . 12_554 ?
C31 P1 C36 23.3(4) 2_665 12_554 ?
C36 P1 C36 115.0(4) 11_564 12_554 ?
C36 P1 C36 115.0(4) 10_454 12_554 ?
C31 P1 P1 64.11(14) 3_565 10_454 ?
C31 P1 P1 64.12(14) . 10_454 ?
C31 P1 P1 64.12(14) 2_665 10_454 ?
C36 P1 P1 76.8(3) 11_564 10_454 ?
C36 P1 P1 76.83(14) 10_454 10_454 ?
C36 P1 P1 76.8(3) 12_554 10_454 ?
C32 C31 C36 120.0 . . ?
C32 C31 P1 113.3(2) . . ?
C36 C31 P1 126.7(2) . . ?
C31 C32 C33 120.0 . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 P1 143.1(3) . 10_454 ?
C31 C36 P1 83.99(18) . 10_454 ?
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
Ni N1 1.633(4) . ?
Ni Se 2.4489(3) 2_665 ?
Ni Se 2.4489(3) . ?
Ni Se 2.4489(3) 3_565 ?
Se C11 1.864(2) . ?
N1 O1 1.156(5) . ?
B N11 1.547(2) 2_665 ?
B N11 1.547(2) 3_565 ?
B N11 1.547(2) . ?
N11 C11 1.351(3) . ?
N11 C12 1.389(3) . ?
N12 C11 1.355(3) . ?
N12 C13 1.386(3) . ?
N12 C21 1.443(3) . ?
C12 C13 1.338(3) . ?
C21 C26 1.378(3) . ?
C21 C22 1.393(3) . ?
C22 C23 1.389(3) . ?
C22 C27 1.496(4) . ?
C23 C24 1.376(4) . ?
C24 C25 1.389(4) . ?
C24 C28 1.516(4) . ?
C25 C26 1.402(3) . ?
C26 C29 1.506(3) . ?
P1 C31 1.819(4) 3_565 ?
P1 C31 1.819(4) . ?
P1 C31 1.819(4) 2_665 ?
P1 C36 2.077(16) 11_564 ?
P1 C36 2.077(5) 10_454 ?
P1 C36 2.077(6) 12_554 ?
P1 P1 2.516(4) 10_454 ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C36 P1 2.077(5) 10_454 ?
