#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:04:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179466 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/63/4336335.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_4336335
loop_
_publ_author_name
'Sergio S. Rozenel'
'Rosa Padilla'
'John Arnold'
_publ_section_title
;
 Chemistry of Reduced Monomeric and Dimeric Cobalt Complexes Supported by
 a PNP Pincer Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11544
_journal_page_last               11550
_journal_paper_doi               10.1021/ic4018882
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C16 H36 Co N3 P2'
_chemical_formula_sum            'C16 H36 Co N3 P2'
_chemical_formula_weight         391.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.2980(10)
_cell_angle_beta                 84.3140(12)
_cell_angle_gamma                68.0490(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6183(7)
_cell_length_b                   8.5862(8)
_cell_length_c                   17.7206(16)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    159(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.36
_cell_volume                     1048.62(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      159(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω 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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16492
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0221
_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)+(0.0305P)²+0.3425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                3649
_reflns_number_total             3845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4018882_si_005.cif
_cod_data_source_block           PNPCoN2
_cod_database_code               4336335
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
Co1 Co 0.49092(2) 0.18569(2) 0.252380(10) 0.02422(7) Uani 1 1 d .
P2 P 0.65845(5) 0.11414(5) 0.15095(2) 0.02551(9) Uani 1 1 d .
P1 P 0.31667(5) 0.30935(5) 0.34272(2) 0.02715(9) Uani 1 1 d .
N1 N 0.32718(17) 0.36436(15) 0.18351(7) 0.0292(3) Uani 1 1 d .
C2 C 0.1138(2) 0.4730(2) 0.28906(9) 0.0389(4) Uani 1 1 d .
H2A H 0.0127 0.4298 0.2898 0.047 Uiso 1 1 calc R
H2B H 0.0663 0.5742 0.3119 0.047 Uiso 1 1 calc R
C9 C 0.3690(2) 0.40850(19) 0.10116(9) 0.0366(4) Uani 1 1 d .
H9A H 0.4275 0.4939 0.0927 0.044 Uiso 1 1 calc R
H9B H 0.2522 0.4573 0.0726 0.044 Uiso 1 1 calc R
C10 C 0.5017(2) 0.25037(19) 0.07135(8) 0.0345(3) Uani 1 1 d .
H10A H 0.5747 0.2830 0.0269 0.041 Uiso 1 1 calc R
H10B H 0.4299 0.1901 0.0562 0.041 Uiso 1 1 calc R
C1 C 0.1836(2) 0.5161(2) 0.20645(9) 0.0384(4) Uani 1 1 d .
H1A H 0.0778 0.5607 0.1716 0.046 Uiso 1 1 calc R
H1B H 0.2368 0.6041 0.2025 0.046 Uiso 1 1 calc R
C12 C 0.5568(2) -0.1635(2) 0.14844(11) 0.0424(4) Uani 1 1 d .
H12A H 0.5951 -0.2793 0.1413 0.064 Uiso 1 1 calc R
H12B H 0.4621 -0.0893 0.1115 0.064 Uiso 1 1 calc R
H12C H 0.5058 -0.1565 0.1999 0.064 Uiso 1 1 calc R
C11 C 0.7283(2) -0.10820(18) 0.13675(8) 0.0304(3) Uani 1 1 d .
H11A H 0.8176 -0.1817 0.1776 0.036 Uiso 1 1 calc R
C3 C 0.4105(2) 0.4244(2) 0.39520(9) 0.0367(3) Uani 1 1 d .
H3A H 0.3062 0.4921 0.4253 0.044 Uiso 1 1 calc R
C6 C 0.2185(2) 0.1825(2) 0.42069(9) 0.0377(4) Uani 1 1 d .
H6A H 0.3238 0.1036 0.4539 0.045 Uiso 1 1 calc R
C14 C 0.8797(2) 0.1581(2) 0.13212(10) 0.0406(4) Uani 1 1 d .
H14A H 0.9295 0.1350 0.0809 0.049 Uiso 1 1 calc R
C13 C 0.8297(2) -0.1392(2) 0.05954(9) 0.0399(4) Uani 1 1 d .
H13A H 0.8627 -0.2571 0.0565 0.060 Uiso 1 1 calc R
H13B H 0.9424 -0.1128 0.0558 0.060 Uiso 1 1 calc R
H13C H 0.7475 -0.0671 0.0178 0.060 Uiso 1 1 calc R
C4 C 0.5629(3) 0.2979(3) 0.45138(11) 0.0507(4) Uani 1 1 d .
H4A H 0.6105 0.3598 0.4779 0.076 Uiso 1 1 calc R
H4B H 0.6645 0.2272 0.4232 0.076 Uiso 1 1 calc R
H4C H 0.5095 0.2271 0.4884 0.076 Uiso 1 1 calc R
C15 C 0.8423(3) 0.3460(3) 0.13205(13) 0.0568(5) Uani 1 1 d .
H15A H 0.9587 0.3665 0.1220 0.085 Uiso 1 1 calc R
H15B H 0.7912 0.3713 0.1816 0.085 Uiso 1 1 calc R
H15C H 0.7534 0.4180 0.0925 0.085 Uiso 1 1 calc R
C16 C 1.0263(3) 0.0400(3) 0.19218(14) 0.0625(6) Uani 1 1 d .
H16A H 1.1408 0.0639 0.1819 0.094 Uiso 1 1 calc R
H16B H 1.0523 -0.0771 0.1896 0.094 Uiso 1 1 calc R
H16C H 0.9783 0.0588 0.2429 0.094 Uiso 1 1 calc R
C7 C 0.1392(3) 0.0734(3) 0.38689(12) 0.0559(5) Uani 1 1 d .
H7A H 0.0890 0.0076 0.4280 0.084 Uiso 1 1 calc R
H7B H 0.2385 -0.0025 0.3600 0.084 Uiso 1 1 calc R
H7C H 0.0404 0.1468 0.3515 0.084 Uiso 1 1 calc R
N3 N 0.7054(3) -0.1206(2) 0.35564(9) 0.0616(5) Uani 1 1 d .
C8 C 0.0710(3) 0.2907(3) 0.47189(10) 0.0500(4) Uani 1 1 d .
H8A H 0.0258 0.2175 0.5113 0.075 Uiso 1 1 calc R
H8B H -0.0330 0.3721 0.4409 0.075 Uiso 1 1 calc R
H8C H 0.1274 0.3504 0.4957 0.075 Uiso 1 1 calc R
C5 C 0.4858(4) 0.5473(3) 0.33812(12) 0.0645(6) Uani 1 1 d .
H5A H 0.5333 0.6066 0.3661 0.097 Uiso 1 1 calc R
H5B H 0.3853 0.6288 0.3053 0.097 Uiso 1 1 calc R
H5C H 0.5859 0.4838 0.3070 0.097 Uiso 1 1 calc R
N2 N 0.62331(19) 0.00140(17) 0.31563(7) 0.0371(3) Uani 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
N2 Co1 N1 171.49(6)
N2 Co1 P2 94.66(4)
N1 Co1 P2 85.66(4)
N2 Co1 P1 94.88(4)
N1 Co1 P1 85.84(4)
P2 Co1 P1 168.537(16)
C10 P2 C14 106.01(8)
C10 P2 C11 106.24(7)
C14 P2 C11 103.72(7)
C10 P2 Co1 102.96(5)
C14 P2 Co1 117.86(5)
C11 P2 Co1 118.90(5)
C2 P1 C6 106.15(8)
C2 P1 C3 105.89(8)
C6 P1 C3 103.34(7)
C2 P1 Co1 102.54(5)
C6 P1 Co1 118.82(6)
C3 P1 Co1 118.84(5)
C9 N1 C1 108.05(11)
C9 N1 Co1 124.09(10)
C1 N1 Co1 123.58(10)
C1 C2 P1 106.68(10)
N1 C9 C10 110.75(12)
C9 C10 P2 106.56(10)
N1 C1 C2 110.89(12)
C13 C11 C12 111.32(13)
C13 C11 P2 114.16(11)
C12 C11 P2 110.27(10)
C4 C3 C5 111.39(16)
C4 C3 P1 110.61(12)
C5 C3 P1 110.37(12)
C8 C6 C7 111.23(14)
C8 C6 P1 113.53(12)
C7 C6 P1 110.16(12)
C16 C14 C15 110.77(16)
C16 C14 P2 110.12(13)
C15 C14 P2 110.67(12)
N3 N2 Co1 177.55(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 N2 1.7402(13)
Co1 N1 1.8566(12)
Co1 P2 2.1637(4)
Co1 P1 2.1737(4)
P2 C10 1.8296(15)
P2 C14 1.8451(16)
P2 C11 1.8484(15)
P1 C2 1.8297(15)
P1 C6 1.8429(16)
P1 C3 1.8481(16)
N1 C9 1.4593(19)
N1 C1 1.4623(19)
C2 C1 1.522(2)
C9 C10 1.526(2)
C12 C11 1.530(2)
C11 C13 1.528(2)
C3 C4 1.526(2)
C3 C5 1.528(2)
C6 C8 1.529(2)
C6 C7 1.531(2)
C14 C16 1.524(3)
C14 C15 1.529(2)
N3 N2 1.1235(19)
