#------------------------------------------------------------------------------
#$Date: 2018-08-20 18:13:25 +0300 (Mon, 20 Aug 2018) $
#$Revision: 209994 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/23/4302309.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_4302309
loop_
_publ_author_name
'Kornev, Alexander N.'
'Belina, Natalia V.'
'Sushev, Vyacheslav V.'
'Fukin, Georgy K.'
'Baranov, Evgenii V.'
'Kurskiy, Yuriy A.'
'Poddelskii, Andrei I.'
'Abakumov, Gleb A.'
'Lönnecke, Peter'
'Hey-Hawkins, Evamarie'
_publ_section_title
;
 The First Structurally Characterized Metal (κ²N,P)-Phosphinohydrazides:
 The Key to Understanding the Intramolecular Rearrangement
 R₂P--NR'--NR'--M →  R'N=PR₂--NR'--M.
 Metalloderivatives of Diisopropylphosphinohydrazines:
 Synthesis and Properties
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5574
_journal_page_last               5583
_journal_paper_doi               10.1021/ic900135b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C36 H48 Co N4 P2'
_chemical_formula_weight         657.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.9040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5386(4)
_cell_length_b                   21.3880(9)
_cell_length_c                   9.5457(4)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     1699.24(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9356
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.8335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         2989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0275
_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)+(0.0478P)²+0.6254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                2798
_reflns_number_total             2989
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338593
_cod_data_source_file            ic900135b_si_001_4.cif
_cod_data_source_block           710338
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      'P 21/c'
_cod_database_code               4302309
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.5000 0.01382(11) Uani 1 2 d S . .
P1 P 0.37087(4) 0.575981(17) 0.36089(4) 0.01423(12) Uani 1 1 d . . .
N1 N 0.44378(15) 0.56269(6) 0.61854(13) 0.0161(3) Uani 1 1 d . . .
C1 C 0.16368(18) 0.57858(7) 0.25158(16) 0.0184(3) Uani 1 1 d . . .
H1 H 0.125(2) 0.6193(9) 0.2703(19) 0.021(4) Uiso 1 1 d . . .
N2 N 0.36553(15) 0.61204(6) 0.52017(13) 0.0160(3) Uani 1 1 d . . .
C2 C 0.1500(2) 0.57254(9) 0.08960(18) 0.0272(4) Uani 1 1 d . . .
H2C H 0.043(3) 0.5783(10) 0.039(2) 0.033(5) Uiso 1 1 d . . .
H2B H 0.176(2) 0.5316(10) 0.064(2) 0.032(5) Uiso 1 1 d . . .
H2A H 0.214(3) 0.6033(10) 0.049(2) 0.038(6) Uiso 1 1 d . . .
C3 C 0.0669(2) 0.52842(10) 0.3085(2) 0.0314(4) Uani 1 1 d . . .
H3C H 0.104(3) 0.4877(11) 0.292(2) 0.036(6) Uiso 1 1 d . . .
H3B H 0.071(3) 0.5332(10) 0.408(3) 0.040(6) Uiso 1 1 d . . .
H3A H -0.046(3) 0.5320(11) 0.260(2) 0.045(6) Uiso 1 1 d . . .
C4 C 0.49688(19) 0.62458(7) 0.27224(17) 0.0191(3) Uani 1 1 d . . .
H4 H 0.497(2) 0.6016(9) 0.187(2) 0.023(4) Uiso 1 1 d . . .
C5 C 0.4375(2) 0.69084(8) 0.2354(2) 0.0296(4) Uani 1 1 d . . .
H5C H 0.329(3) 0.6932(9) 0.185(2) 0.033(5) Uiso 1 1 d . . .
H5B H 0.453(2) 0.7158(10) 0.323(2) 0.036(6) Uiso 1 1 d . . .
H5A H 0.502(3) 0.7101(10) 0.174(2) 0.041(6) Uiso 1 1 d . . .
C6 C 0.6682(2) 0.62432(9) 0.3655(2) 0.0268(4) Uani 1 1 d . . .
H6C H 0.741(2) 0.6480(10) 0.322(2) 0.034(5) Uiso 1 1 d . . .
H6B H 0.669(2) 0.6405(9) 0.460(2) 0.029(5) Uiso 1 1 d . . .
H6A H 0.717(2) 0.5806(10) 0.382(2) 0.035(5) Uiso 1 1 d . . .
C7 C 0.53903(17) 0.58920(7) 0.74393(16) 0.0159(3) Uani 1 1 d . . .
C8 C 0.58765(18) 0.65200(7) 0.75501(17) 0.0192(3) Uani 1 1 d . . .
H8 H 0.554(2) 0.6781(8) 0.6764(19) 0.016(4) Uiso 1 1 d . . .
C9 C 0.68247(19) 0.67476(8) 0.88204(17) 0.0215(3) Uani 1 1 d . . .
H9 H 0.718(2) 0.7187(9) 0.8867(18) 0.019(4) Uiso 1 1 d . . .
C10 C 0.73029(19) 0.63663(8) 1.00071(17) 0.0221(3) Uani 1 1 d . . .
H10 H 0.797(2) 0.6531(9) 1.085(2) 0.033(5) Uiso 1 1 d . . .
C11 C 0.67824(19) 0.57497(8) 0.99207(17) 0.0215(3) Uani 1 1 d . . .
H11 H 0.704(2) 0.5491(9) 1.072(2) 0.025(5) Uiso 1 1 d . . .
C12 C 0.58312(18) 0.55163(8) 0.86658(17) 0.0189(3) Uani 1 1 d . . .
H12 H 0.544(2) 0.5097(9) 0.8630(19) 0.018(4) Uiso 1 1 d . . .
C13 C 0.23440(17) 0.64307(7) 0.55829(16) 0.0167(3) Uani 1 1 d . . .
C14 C 0.16768(19) 0.62151(8) 0.67033(17) 0.0208(3) Uani 1 1 d . . .
H14 H 0.212(2) 0.5847(9) 0.722(2) 0.028(5) Uiso 1 1 d . . .
C15 C 0.0419(2) 0.65372(8) 0.70717(18) 0.0245(4) Uani 1 1 d . . .
H15 H -0.001(2) 0.6386(9) 0.780(2) 0.025(5) Uiso 1 1 d . . .
C16 C -0.0184(2) 0.70796(8) 0.63565(18) 0.0240(4) Uani 1 1 d . . .
H16 H -0.104(2) 0.7296(9) 0.663(2) 0.027(5) Uiso 1 1 d . . .
C17 C 0.0486(2) 0.72983(8) 0.52557(18) 0.0216(3) Uani 1 1 d . . .
H17 H 0.012(2) 0.7671(9) 0.4776(18) 0.018(4) Uiso 1 1 d . . .
C18 C 0.17429(18) 0.69812(7) 0.48729(17) 0.0191(3) Uani 1 1 d . . .
H18 H 0.224(2) 0.7140(9) 0.414(2) 0.023(4) Uiso 1 1 d . . .
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'
Co Co 0.3494 0.9721 '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 Co1 N1 180.0 . 3_666 ?
N1 Co1 P1 71.36(4) . . ?
N1 Co1 P1 108.64(4) 3_666 . ?
N1 Co1 P1 108.64(4) . 3_666 ?
N1 Co1 P1 71.36(4) 3_666 3_666 ?
P1 Co1 P1 180.0 . 3_666 ?
N2 P1 C4 106.79(7) . . ?
N2 P1 C1 106.03(7) . . ?
C4 P1 C1 108.04(7) . . ?
N2 P1 Co1 84.68(4) . . ?
C4 P1 Co1 115.17(5) . . ?
C1 P1 Co1 130.09(5) . . ?
C7 N1 N2 110.35(11) . . ?
C7 N1 Co1 128.39(10) . . ?
N2 N1 Co1 105.53(8) . . ?
C3 C1 C2 112.05(15) . . ?
C3 C1 P1 107.74(11) . . ?
C2 C1 P1 114.63(11) . . ?
C13 N2 N1 116.40(11) . . ?
C13 N2 P1 128.13(10) . . ?
N1 N2 P1 98.34(8) . . ?
C5 C4 C6 111.31(14) . . ?
C5 C4 P1 115.84(12) . . ?
C6 C4 P1 108.19(11) . . ?
C12 C7 C8 117.82(14) . . ?
C12 C7 N1 118.44(13) . . ?
C8 C7 N1 123.70(14) . . ?
C9 C8 C7 120.47(15) . . ?
C10 C9 C8 121.17(15) . . ?
C9 C10 C11 118.69(15) . . ?
C12 C11 C10 120.87(16) . . ?
C11 C12 C7 120.90(15) . . ?
C18 C13 C14 118.73(14) . . ?
C18 C13 N2 119.70(14) . . ?
C14 C13 N2 121.50(14) . . ?
C15 C14 C13 120.11(15) . . ?
C16 C15 C14 121.02(16) . . ?
C15 C16 C17 119.01(15) . . ?
C16 C17 C18 120.68(15) . . ?
C17 C18 C13 120.43(15) . . ?
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
Co1 N1 1.8844(12) . ?
Co1 N1 1.8844(12) 3_666 ?
Co1 P1 2.2285(4) . ?
Co1 P1 2.2285(4) 3_666 ?
P1 N2 1.7146(13) . ?
P1 C4 1.8333(16) . ?
P1 C1 1.8432(15) . ?
N1 C7 1.4075(19) . ?
N1 N2 1.4704(17) . ?
C1 C3 1.526(2) . ?
C1 C2 1.530(2) . ?
N2 C13 1.4172(19) . ?
C4 C5 1.520(2) . ?
C4 C6 1.533(2) . ?
C7 C12 1.400(2) . ?
C7 C8 1.403(2) . ?
C8 C9 1.387(2) . ?
C9 C10 1.381(2) . ?
C10 C11 1.388(2) . ?
C11 C12 1.382(2) . ?
C13 C18 1.398(2) . ?
C13 C14 1.397(2) . ?
C14 C15 1.385(2) . ?
C15 C16 1.386(2) . ?
C16 C17 1.385(2) . ?
C17 C18 1.386(2) . ?
