#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:04:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179438 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/35/4333550.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_4333550
loop_
_publ_author_name
'Ramyaa Mathialagan'
'Subramaniam Kuppuswamy'
'Alexandra T. De Denko'
'Mark W. Bezpalko'
'Bruce M. Foxman'
'Christine M. Thomas'
_publ_contact_author_address
;Brandeis University
Dept. of Chemistry    
415 South St MS 015    
Waltham, MA 02454    
;
_publ_contact_author_email       thomasc@brandeis.edu
_publ_contact_author_name        'Christine M. Thomas'
_publ_section_title
;
 Metal-Metal Bonding in Low-Coordinate Dicobalt Complexes Supported by
 Phosphinoamide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              701
_journal_page_last               706
_journal_paper_doi               10.1021/ic3018375
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C36 H68 Co2 N2 P4'
_chemical_formula_sum            'C36 H68 Co2 N2 P4'
_chemical_formula_weight         770.71
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2012-06-16
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                106.184(2)
_cell_angle_beta                 105.840(2)
_cell_angle_gamma                110.519(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7710(5)
_cell_length_b                   11.5687(6)
_cell_length_c                   12.0272(6)
_cell_measurement_reflns_used    9347
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1000.13(10)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31883
_diffrn_reflns_theta_full        29.459
_diffrn_reflns_theta_max         30.060
_diffrn_reflns_theta_min         1.935
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       prism
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5836
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.0002353
_refine_ls_shift/su_mean         0.0000167
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 0.39P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0524
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0524
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5439
_reflns_number_total             5836
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0221
_oxford_refine_ls_scale          0.24379(9)
_oxford_reflns_number_all        5836
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'RM_106_0m in P-1'
_cod_data_source_file            ic3018375_si_002_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4333550
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT CO   (    1 ,X'S,U'S)  UNTIL C    (   18 ) 
CONT H    (   11 ,X'S,U[ISO])  UNTIL H    (  183 ) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
#END Tags that were not found in dictionaries
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_occupancy
_atom_site_adp_type
Co1 Co -0.063449(16) -0.049020(12) -0.121161(12) 0.0122 1.0000 Uani
P1 P 0.15266(3) 0.20906(2) 0.05728(2) 0.0126 1.0000 Uani
P2 P -0.08963(4) -0.14463(3) -0.32224(2) 0.0177 1.0000 Uani
N1 N 0.04666(11) 0.13963(8) -0.09932(8) 0.0147 1.0000 Uani
C1 C 0.39850(13) 0.28525(10) 0.09960(10) 0.0176 1.0000 Uani
C2 C 0.50900(15) 0.35509(13) 0.24337(11) 0.0258 1.0000 Uani
C3 C 0.44820(15) 0.17787(12) 0.03640(12) 0.0244 1.0000 Uani
C4 C 0.13154(14) 0.36511(10) 0.12812(10) 0.0171 1.0000 Uani
C5 C 0.20557(16) 0.48035(11) 0.08815(11) 0.0214 1.0000 Uani
C6 C -0.06134(15) 0.32952(11) 0.10935(11) 0.0224 1.0000 Uani
C7 C -0.02523(13) 0.18853(9) -0.18449(9) 0.0148 1.0000 Uani
C8 C 0.07767(13) 0.27277(10) -0.22903(9) 0.0169 1.0000 Uani
C9 C -0.00573(15) 0.31190(10) -0.31783(10) 0.0202 1.0000 Uani
C10 C -0.18839(16) 0.26853(11) -0.36772(10) 0.0219 1.0000 Uani
C11 C -0.28993(15) 0.18232(11) -0.32616(10) 0.0213 1.0000 Uani
C12 C -0.21237(13) 0.14220(10) -0.23671(10) 0.0173 1.0000 Uani
C13 C 0.27578(14) 0.32144(11) -0.18471(11) 0.0215 1.0000 Uani
C14 C -0.2747(2) 0.31167(14) -0.46409(12) 0.0318 1.0000 Uani
C15 C -0.33012(14) 0.04488(11) -0.19941(11) 0.0220 1.0000 Uani
C16 C -0.1928(2) -0.10038(14) -0.44765(11) 0.0309 1.0000 Uani
C17 C -0.1859(2) -0.32761(12) -0.41553(12) 0.0331 1.0000 Uani
C18 C 0.13449(17) -0.08874(14) -0.31936(12) 0.0300 1.0000 Uani
H11 H 0.4265(18) 0.3535(14) 0.0673(14) 0.023(3) 1.0000 Uiso
H21 H 0.497(2) 0.4328(16) 0.2862(15) 0.030(4) 1.0000 Uiso
H22 H 0.476(2) 0.2938(16) 0.2818(15) 0.030(4) 1.0000 Uiso
H23 H 0.633(2) 0.3851(17) 0.2610(16) 0.041(4) 1.0000 Uiso
H31 H 0.565(2) 0.2194(17) 0.0413(16) 0.039(4) 1.0000 Uiso
H32 H 0.444(2) 0.1190(17) 0.0790(16) 0.040(4) 1.0000 Uiso
H33 H 0.370(2) 0.1249(15) -0.0524(15) 0.029(4) 1.0000 Uiso
H41 H 0.2036(18) 0.3968(14) 0.2182(13) 0.022(3) 1.0000 Uiso
H51 H 0.331(2) 0.5109(14) 0.1064(14) 0.026(4) 1.0000 Uiso
H52 H 0.141(2) 0.4510(15) -0.0019(15) 0.029(4) 1.0000 Uiso
H53 H 0.195(2) 0.5598(16) 0.1344(15) 0.031(4) 1.0000 Uiso
H61 H -0.065(2) 0.4051(16) 0.1656(15) 0.035(4) 1.0000 Uiso
H62 H -0.115(2) 0.2533(15) 0.1294(14) 0.030(4) 1.0000 Uiso
H63 H -0.135(2) 0.3083(15) 0.0236(15) 0.027(4) 1.0000 Uiso
H91 H 0.0694(19) 0.3726(15) -0.3447(14) 0.027(4) 1.0000 Uiso
H111 H -0.414(2) 0.1514(15) -0.3572(15) 0.030(4) 1.0000 Uiso
H131 H 0.315(2) 0.3392(16) -0.2481(15) 0.035(4) 1.0000 Uiso
H132 H 0.311(2) 0.2547(16) -0.1659(15) 0.033(4) 1.0000 Uiso
H133 H 0.342(2) 0.4056(16) -0.1085(15) 0.032(4) 1.0000 Uiso
H141 H -0.185(3) 0.3724(19) -0.4815(18) 0.051(5) 1.0000 Uiso
H142 H -0.367(3) 0.2338(19) -0.5423(19) 0.051(5) 1.0000 Uiso
H143 H -0.336(2) 0.3581(19) -0.4313(18) 0.049(5) 1.0000 Uiso
H151 H -0.296(2) 0.0796(17) -0.1085(16) 0.038(4) 1.0000 Uiso
H152 H -0.451(2) 0.0253(17) -0.2375(17) 0.042(5) 1.0000 Uiso
H153 H -0.323(2) -0.0401(17) -0.2237(16) 0.039(4) 1.0000 Uiso
H161 H -0.138(2) -0.0045(19) -0.4205(17) 0.046(5) 1.0000 Uiso
H162 H -0.179(2) -0.1426(17) -0.5247(17) 0.040(4) 1.0000 Uiso
H163 H -0.317(3) -0.1313(19) -0.4655(18) 0.050(5) 1.0000 Uiso
H171 H -0.115(2) -0.3620(17) -0.3725(16) 0.039(4) 1.0000 Uiso
H172 H -0.183(2) -0.3443(17) -0.4979(17) 0.041(4) 1.0000 Uiso
H173 H -0.311(3) -0.3724(19) -0.4288(18) 0.054(5) 1.0000 Uiso
H181 H 0.193(2) 0.0107(19) -0.2838(17) 0.047(5) 1.0000 Uiso
H182 H 0.202(2) -0.1173(18) -0.2647(17) 0.044(5) 1.0000 Uiso
H183 H 0.129(2) -0.1261(17) -0.4039(17) 0.041(4) 1.0000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Co1 2_555 Co1 P1 2_555 69.436(9) yes
Co1 2_555 Co1 P1 . 48.715(7) yes
P1 2_555 Co1 P1 . 118.151(9) yes
Co1 2_555 Co1 P2 . 160.244(11) yes
P1 2_555 Co1 P2 . 108.440(12) yes
P1 . Co1 P2 . 129.229(10) yes
Co1 2_555 Co1 N1 . 85.68(3) yes
P1 2_555 Co1 N1 . 154.62(3) yes
P1 . Co1 N1 . 37.25(2) yes
P2 . Co1 N1 . 96.66(3) yes
Co1 . P1 Co1 2_555 61.849(9) yes
Co1 . P1 N1 . 45.75(3) yes
Co1 2_555 P1 N1 . 107.19(3) yes
Co1 . P1 C1 . 119.40(3) yes
Co1 2_555 P1 C1 . 112.46(3) yes
N1 . P1 C1 . 108.12(4) yes
Co1 . P1 C4 . 137.66(3) yes
Co1 2_555 P1 C4 . 117.80(3) yes
N1 . P1 C4 . 110.63(4) yes
C1 . P1 C4 . 100.27(5) yes
Co1 . P2 C16 . 121.37(4) yes
Co1 . P2 C17 . 124.41(4) yes
C16 . P2 C17 . 98.58(7) yes
Co1 . P2 C18 . 108.40(4) yes
C16 . P2 C18 . 99.66(7) yes
C17 . P2 C18 . 100.04(7) yes
Co1 . N1 P1 . 97.01(4) yes
Co1 . N1 C7 . 124.04(6) yes
P1 . N1 C7 . 131.73(7) yes
P1 . C1 C2 . 112.17(7) yes
P1 . C1 C3 . 110.68(7) yes
C2 . C1 C3 . 110.80(9) yes
P1 . C1 H11 . 107.3(8) no
C2 . C1 H11 . 107.4(8) no
C3 . C1 H11 . 108.3(8) no
C1 . C2 H21 . 114.2(9) no
C1 . C2 H22 . 110.8(9) no
H21 . C2 H22 . 106.4(13) no
C1 . C2 H23 . 109.6(10) no
H21 . C2 H23 . 107.4(13) no
H22 . C2 H23 . 108.2(13) no
C1 . C3 H31 . 110.5(10) no
C1 . C3 H32 . 109.8(10) no
H31 . C3 H32 . 108.1(14) no
C1 . C3 H33 . 112.0(9) no
H31 . C3 H33 . 106.9(13) no
H32 . C3 H33 . 109.4(13) no
P1 . C4 C5 . 117.07(7) yes
P1 . C4 C6 . 110.86(7) yes
C5 . C4 C6 . 110.17(9) yes
P1 . C4 H41 . 101.7(8) no
C5 . C4 H41 . 108.0(8) no
C6 . C4 H41 . 108.4(8) no
C4 . C5 H51 . 112.0(9) no
C4 . C5 H52 . 110.4(9) no
H51 . C5 H52 . 108.4(12) no
C4 . C5 H53 . 110.9(9) no
H51 . C5 H53 . 106.5(12) no
H52 . C5 H53 . 108.5(12) no
C4 . C6 H61 . 109.8(9) no
C4 . C6 H62 . 112.5(9) no
H61 . C6 H62 . 106.2(13) no
C4 . C6 H63 . 111.5(9) no
H61 . C6 H63 . 108.2(13) no
H62 . C6 H63 . 108.4(12) no
N1 . C7 C8 . 123.25(9) yes
N1 . C7 C12 . 118.75(8) yes
C8 . C7 C12 . 117.78(9) yes
C7 . C8 C9 . 119.57(9) yes
C7 . C8 C13 . 121.93(9) yes
C9 . C8 C13 . 118.49(9) yes
C8 . C9 C10 . 122.81(10) yes
C8 . C9 H91 . 117.7(9) no
C10 . C9 H91 . 119.5(9) no
C9 . C10 C11 . 117.35(9) yes
C9 . C10 C14 . 121.59(11) yes
C11 . C10 C14 . 121.05(11) yes
C10 . C11 C12 . 121.80(10) yes
C10 . C11 H111 . 119.8(9) no
C12 . C11 H111 . 118.3(9) no
C7 . C12 C11 . 120.63(9) yes
C7 . C12 C15 . 120.15(9) yes
C11 . C12 C15 . 119.18(9) yes
C8 . C13 H131 . 110.7(10) no
C8 . C13 H132 . 112.1(9) no
H131 . C13 H132 . 107.9(13) no
C8 . C13 H133 . 111.2(9) no
H131 . C13 H133 . 106.9(13) no
H132 . C13 H133 . 107.8(13) no
C10 . C14 H141 . 110.5(11) no
C10 . C14 H142 . 111.8(11) no
H141 . C14 H142 . 111.0(15) no
C10 . C14 H143 . 109.4(11) no
H141 . C14 H143 . 108.9(15) no
H142 . C14 H143 . 105.2(15) no
C12 . C15 H151 . 112.4(10) no
C12 . C15 H152 . 111.8(10) no
H151 . C15 H152 . 106.9(14) no
C12 . C15 H153 . 110.9(10) no
H151 . C15 H153 . 106.2(13) no
H152 . C15 H153 . 108.3(14) no
P2 . C16 H161 . 110.3(11) no
P2 . C16 H162 . 109.7(10) no
H161 . C16 H162 . 109.4(14) no
P2 . C16 H163 . 109.5(11) no
H161 . C16 H163 . 108.0(15) no
H162 . C16 H163 . 110.0(15) no
P2 . C17 H171 . 108.9(10) no
P2 . C17 H172 . 109.7(10) no
H171 . C17 H172 . 108.2(14) no
P2 . C17 H173 . 109.7(11) no
H171 . C17 H173 . 112.4(15) no
H172 . C17 H173 . 107.9(15) no
P2 . C18 H181 . 107.5(10) no
P2 . C18 H182 . 109.7(10) no
H181 . C18 H182 . 108.7(14) no
P2 . C18 H183 . 111.1(10) no
H181 . C18 H183 . 110.5(14) no
H182 . C18 H183 . 109.2(14) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 Co1 2_555 2.5536(3) yes
Co1 P1 2_555 2.1763(3) yes
Co1 P1 . 2.7116(3) yes
Co1 P2 . 2.2699(3) yes
Co1 N1 . 1.9569(8) yes
P1 N1 . 1.6535(9) yes
P1 C1 . 1.8718(10) yes
P1 C4 . 1.8661(10) yes
P2 C16 . 1.8346(13) yes
P2 C17 . 1.8327(12) yes
P2 C18 . 1.8283(12) yes
N1 C7 . 1.4097(12) yes
C1 C2 . 1.5295(15) yes
C1 C3 . 1.5314(16) yes
C1 H11 . 0.961(14) no
C2 H21 . 0.963(16) no
C2 H22 . 0.956(16) no
C2 H23 . 0.956(17) no
C3 H31 . 0.946(17) no
C3 H32 . 0.956(17) no
C3 H33 . 0.963(16) no
C4 C5 . 1.5333(14) yes
C4 C6 . 1.5277(15) yes
C4 H41 . 0.974(14) no
C5 H51 . 0.967(15) no
C5 H52 . 0.966(15) no
C5 H53 . 0.983(16) no
C6 H61 . 0.961(16) no
C6 H62 . 0.973(15) no
C6 H63 . 0.962(15) no
C7 C8 . 1.4105(13) yes
C7 C12 . 1.4173(14) yes
C8 C9 . 1.3985(14) yes
C8 C13 . 1.5039(15) yes
C9 C10 . 1.3865(16) yes
C9 H91 . 0.975(15) no
C10 C11 . 1.3914(16) yes
C10 C14 . 1.5078(15) yes
C11 C12 . 1.3914(14) yes
C11 H111 . 0.936(15) no
C12 C15 . 1.5016(14) yes
C13 H131 . 0.959(16) no
C13 H132 . 0.984(16) no
C13 H133 . 0.970(16) no
C14 H141 . 0.967(19) no
C14 H142 . 0.976(19) no
C14 H143 . 0.966(19) no
C15 H151 . 0.968(17) no
C15 H152 . 0.942(18) no
C15 H153 . 0.974(17) no
C16 H161 . 0.952(18) no
C16 H162 . 0.982(18) no
C16 H163 . 0.955(19) no
C17 H171 . 0.961(17) no
C17 H172 . 0.965(18) no
C17 H173 . 0.98(2) no
C18 H181 . 0.980(18) no
C18 H182 . 0.970(18) no
C18 H183 . 0.969(17) no
