#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:34:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179754 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/50/7005097.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_7005097
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            'C15 H22 B N7 Ni O'
_chemical_formula_weight         385.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           26
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2'
_symmetry_space_group_name_H-M   'P m c 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1151(8)
_cell_length_b                   8.0075(5)
_cell_length_c                   17.4989(11)
_cell_measurement_reflns_used    3977
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.54
_cell_volume                     1837.7(2)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12505
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.9002
_exptl_absorpt_correction_T_min  0.9002
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0413P)²+1.2391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                2946
_reflns_number_total             3957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b616674a.txt
_cod_data_source_block           tpnis10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_sg_symbol_H-M      Pmc2(1)
_cod_database_code               7005097
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-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_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
Ni1 Ni 0.5000 0.34336(9) 0.18993(3) 0.0286(2) Uani 1 2 d S . .
Ni2 Ni 0.0000 0.85349(9) 0.21710(4) 0.0298(2) Uani 1 2 d S . .
N1 N 0.5000 0.2740(7) 0.1030(3) 0.0378(12) Uani 1 2 d S . .
N2 N 0.0000 0.8967(7) 0.3074(3) 0.0431(14) Uani 1 2 d S . .
O1 O 0.5000 0.2202(8) 0.0409(3) 0.0795(19) Uani 1 2 d S . .
O2 O 0.0000 0.9159(10) 0.3730(4) 0.110(3) Uani 1 2 d S . .
B1 B 0.5000 0.4603(9) 0.3563(4) 0.0330(16) Uani 1 2 d S . .
H1 H 0.5000 0.501(6) 0.411(3) 0.013(13) Uiso 1 2 d S . .
B2 B 0.0000 0.7493(9) 0.0485(5) 0.0311(18) Uani 1 2 d S . .
H2 H 0.0000 0.710(6) -0.015(3) 0.015(14) Uiso 1 2 d S . .
N11 N 0.5000 0.1947(6) 0.2821(3) 0.0328(12) Uani 1 2 d S . .
N12 N 0.5000 0.2682(7) 0.3516(3) 0.0333(13) Uani 1 2 d S . .
N21 N 0.3941(2) 0.4856(4) 0.23748(18) 0.0291(7) Uani 1 1 d . . .
N22 N 0.4036(2) 0.5239(4) 0.31359(18) 0.0294(7) Uani 1 1 d . . .
N31 N 0.0000 0.6168(5) 0.1797(3) 0.0316(10) Uani 1 2 d S . .
N32 N 0.0000 0.5922(6) 0.1028(3) 0.0291(11) Uani 1 2 d S . .
N41 N 0.1069(2) 0.9158(4) 0.1405(2) 0.0317(7) Uani 1 1 d . . .
N42 N 0.0958(2) 0.8536(4) 0.06812(19) 0.0337(7) Uani 1 1 d . . .
C14 C 0.5000 -0.0920(8) 0.2294(5) 0.052(2) Uani 1 2 d S . .
H14A H 0.5000 -0.0320 0.1812 0.078 Uiso 1 2 calc SR . .
H14B H 0.4396 -0.1616 0.2325 0.078 Uiso 0.50 1 calc PR . .
H14C H 0.5604 -0.1616 0.2325 0.078 Uiso 0.50 1 calc PR . .
C11 C 0.5000 0.0279(8) 0.2929(4) 0.0404(17) Uani 1 2 d S . .
C12 C 0.5000 0.0003(8) 0.3721(4) 0.0463(17) Uani 1 2 d S . .
H12A H 0.5000 -0.1043 0.3964 0.056 Uiso 1 2 calc SR . .
C13 C 0.5000 0.1488(8) 0.4067(4) 0.0394(16) Uani 1 2 d S . .
C15 C 0.5000 0.1947(10) 0.4908(4) 0.055(2) Uani 1 2 d S . .
H15A H 0.5000 0.0937 0.5214 0.083 Uiso 1 2 calc SR . .
H15B H 0.4396 0.2599 0.5024 0.083 Uiso 0.50 1 calc PR . .
H15C H 0.5604 0.2599 0.5024 0.083 Uiso 0.50 1 calc PR . .
C24 C 0.2716(3) 0.5330(6) 0.1328(3) 0.0465(12) Uani 1 1 d . . .
H24A H 0.3231 0.4724 0.1044 0.070 Uiso 1 1 calc R . .
H24B H 0.2624 0.6428 0.1105 0.070 Uiso 1 1 calc R . .
H24C H 0.2076 0.4722 0.1308 0.070 Uiso 1 1 calc R . .
C21 C 0.3047(3) 0.5507(4) 0.2140(3) 0.0326(9) Uani 1 1 d . . .
C22 C 0.2570(3) 0.6269(5) 0.2756(3) 0.0408(11) Uani 1 1 d . . .
H22A H 0.1936 0.6814 0.2750 0.049 Uiso 1 1 calc R . .
C23 C 0.3197(3) 0.6076(5) 0.3373(3) 0.0343(9) Uani 1 1 d . . .
C25 C 0.3043(4) 0.6618(7) 0.4185(3) 0.0549(13) Uani 1 1 d . . .
H25A H 0.3631 0.6296 0.4488 0.082 Uiso 1 1 calc R . .
H25B H 0.2437 0.6087 0.4390 0.082 Uiso 1 1 calc R . .
H25C H 0.2962 0.7821 0.4203 0.082 Uiso 1 1 calc R . .
C34 C 0.0000 0.4461(9) 0.2970(4) 0.0495(18) Uani 1 2 d S . .
H34A H 0.0000 0.5554 0.3209 0.074 Uiso 1 2 calc SR . .
H34B H 0.0604 0.3851 0.3127 0.074 Uiso 0.50 1 calc PR . .
H34C H -0.0604 0.3851 0.3127 0.074 Uiso 0.50 1 calc PR . .
C31 C 0.0000 0.4657(7) 0.2115(4) 0.0392(15) Uani 1 2 d S . .
C32 C 0.0000 0.3446(8) 0.1560(4) 0.0422(18) Uani 1 2 d S . .
H32A H 0.0000 0.2285 0.1638 0.051 Uiso 1 2 calc SR . .
C33 C 0.0000 0.4260(8) 0.0864(4) 0.0351(14) Uani 1 2 d S . .
C35 C 0.0000 0.3570(9) 0.0092(4) 0.0545(19) Uani 1 2 d S . .
H35A H 0.0000 0.4475 -0.0277 0.082 Uiso 1 2 calc SR . .
H35B H -0.0604 0.2889 0.0020 0.082 Uiso 0.50 1 calc PR . .
H35C H 0.0604 0.2889 0.0020 0.082 Uiso 0.50 1 calc PR . .
C44 C 0.2283(3) 1.0853(6) 0.2154(3) 0.0511(13) Uani 1 1 d . . .
H44A H 0.1786 1.0655 0.2554 0.077 Uiso 1 1 calc R . .
H44B H 0.2344 1.2044 0.2064 0.077 Uiso 1 1 calc R . .
H44C H 0.2939 1.0408 0.2309 0.077 Uiso 1 1 calc R . .
C41 C 0.1941(3) 1.0004(5) 0.1432(3) 0.0383(10) Uani 1 1 d . . .
C42 C 0.2395(3) 0.9938(6) 0.0722(3) 0.0471(11) Uani 1 1 d . . .
H42A H 0.3013 1.0447 0.0581 0.057 Uiso 1 1 calc R . .
C43 C 0.1778(3) 0.8992(5) 0.0257(3) 0.0394(10) Uani 1 1 d . . .
C45 C 0.1922(4) 0.8449(7) -0.0555(3) 0.0574(13) Uani 1 1 d . . .
H45C H 0.1341 0.7787 -0.0715 0.086 Uiso 1 1 calc R . .
H45D H 0.2538 0.7783 -0.0595 0.086 Uiso 1 1 calc R . .
H45A H 0.1982 0.9425 -0.0880 0.086 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
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'
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 Ni1 N21 126.32(14) . 4_655 ?
N1 Ni1 N21 126.32(14) . . ?
N21 Ni1 N21 89.11(18) 4_655 . ?
N1 Ni1 N11 123.5(2) . . ?
N21 Ni1 N11 90.21(14) 4_655 . ?
N21 Ni1 N11 90.21(14) . . ?
N2 Ni2 N41 126.88(14) . 4 ?
N2 Ni2 N41 126.88(14) . . ?
N41 Ni2 N41 88.90(19) 4 . ?
N2 Ni2 N31 121.4(3) . . ?
N41 Ni2 N31 90.99(14) 4 . ?
N41 Ni2 N31 90.99(14) . . ?
O1 N1 Ni1 178.5(6) . . ?
O2 N2 Ni2 175.3(7) . . ?
N12 B1 N22 107.5(3) . . ?
N12 B1 N22 107.5(3) . 4_655 ?
N22 B1 N22 108.8(5) . 4_655 ?
N42 B2 N42 108.6(5) . 4 ?
N42 B2 N32 107.3(4) . . ?
N42 B2 N32 107.3(4) 4 . ?
C11 N11 N12 107.7(5) . . ?
C11 N11 Ni1 134.5(5) . . ?
N12 N11 Ni1 117.8(4) . . ?
N11 N12 C13 109.5(6) . . ?
N11 N12 B1 118.9(5) . . ?
C13 N12 B1 131.6(6) . . ?
C21 N21 N22 106.8(3) . . ?
C21 N21 Ni1 134.8(3) . . ?
N22 N21 Ni1 118.2(2) . . ?
C23 N22 N21 109.5(3) . . ?
C23 N22 B1 132.5(4) . . ?
N21 N22 B1 117.9(3) . . ?
C31 N31 N32 106.4(5) . . ?
C31 N31 Ni2 136.2(5) . . ?
N32 N31 Ni2 117.4(4) . . ?
N31 N32 C33 110.4(5) . . ?
N31 N32 B2 118.7(5) . . ?
C33 N32 B2 130.8(6) . . ?
C41 N41 N42 108.0(3) . . ?
C41 N41 Ni2 134.9(3) . . ?
N42 N41 Ni2 117.0(2) . . ?
C43 N42 N41 108.9(3) . . ?
C43 N42 B2 131.9(4) . . ?
N41 N42 B2 119.2(4) . . ?
N11 C11 C12 107.1(6) . . ?
N11 C11 C14 122.7(7) . . ?
C12 C11 C14 130.1(6) . . ?
C13 C12 C11 108.0(6) . . ?
C12 C13 N12 107.7(6) . . ?
C12 C13 C15 131.1(6) . . ?
N12 C13 C15 121.2(6) . . ?
N21 C21 C22 108.9(4) . . ?
N21 C21 C24 120.5(4) . . ?
C22 C21 C24 130.6(4) . . ?
C23 C22 C21 107.1(3) . . ?
N22 C23 C22 107.6(4) . . ?
N22 C23 C25 122.9(4) . . ?
C22 C23 C25 129.4(4) . . ?
N31 C31 C32 110.2(6) . . ?
N31 C31 C34 120.7(6) . . ?
C32 C31 C34 129.1(6) . . ?
C31 C32 C33 106.9(6) . . ?
N32 C33 C32 106.0(6) . . ?
N32 C33 C35 124.4(6) . . ?
C32 C33 C35 129.6(6) . . ?
N41 C41 C42 108.6(4) . . ?
N41 C41 C44 121.1(4) . . ?
C42 C41 C44 130.3(4) . . ?
C43 C42 C41 107.5(4) . . ?
N42 C43 C42 107.0(4) . . ?
N42 C43 C45 122.7(4) . . ?
C42 C43 C45 130.3(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
Ni1 N1 1.619(6) . ?
Ni1 N21 1.980(3) 4_655 ?
Ni1 N21 1.980(3) . ?
Ni1 N11 2.004(5) . ?
Ni2 N2 1.617(6) . ?
Ni2 N41 2.003(3) 4 ?
Ni2 N41 2.003(3) . ?
Ni2 N31 2.006(4) . ?
N1 O1 1.170(7) . ?
N2 O2 1.158(7) . ?
B1 N12 1.541(9) . ?
B1 N22 1.555(5) . ?
B1 N22 1.555(5) 4_655 ?
B2 N42 1.547(6) . ?
B2 N42 1.547(6) 4 ?
B2 N32 1.576(9) . ?
N11 C11 1.349(7) . ?
N11 N12 1.351(7) . ?
N12 C13 1.359(8) . ?
N21 C21 1.348(5) . ?
N21 N22 1.372(4) . ?
N22 C23 1.353(5) . ?
N31 C31 1.331(7) . ?
N31 N32 1.360(7) . ?
N32 C33 1.362(7) . ?
N41 C41 1.330(5) . ?
N41 N42 1.370(5) . ?
N42 C43 1.356(5) . ?
C14 C11 1.469(10) . ?
C11 C12 1.403(9) . ?
C12 C13 1.335(10) . ?
C13 C15 1.517(10) . ?
C24 C21 1.491(6) . ?
C21 C22 1.388(6) . ?
C22 C23 1.366(6) . ?
C23 C25 1.500(6) . ?
C34 C31 1.505(9) . ?
C31 C32 1.373(9) . ?
C32 C33 1.381(9) . ?
C33 C35 1.460(9) . ?
C44 C41 1.502(6) . ?
C41 C42 1.379(6) . ?
C42 C43 1.374(6) . ?
C43 C45 1.498(6) . ?
