#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/25/4302567.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_4302567
loop_
_publ_author_name
'Bennett P. Greenwood'
'Scott I. Forman'
'Gerard T. Rowe'
'Chun-Hsing Chen'
'Bruce M. Foxman'
'Christine M. Thomas'
_publ_section_title
;
Multielectron Redox Activity Facilitated by Metal-Metal Interactions in
Early/Late Heterobimetallics: Co/Zr Complexes Supported by Phosphinoamide
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6251
_journal_page_last               6260
_journal_paper_doi               10.1021/ic900552b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C45 H54 Co1 I1 N3 P3'
_chemical_formula_sum            'C45 H54 Co I N3 P3'
_chemical_formula_weight         915.70
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_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
_audit_creation_date             09-02-16
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   14.8343(4)
_cell_length_b                   14.8343(4)
_cell_length_c                   74.260(2)
_cell_measurement_reflns_used    9191
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     14152.1(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_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  0.031
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       104
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4666
_diffrn_reflns_theta_full        30.193
_diffrn_reflns_theta_max         30.193
_diffrn_reflns_theta_min         1.645
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         4666
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.000916
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² +29.02P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0662
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0662
_reflns_limit_h_max              0
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              104
_reflns_limit_l_min              0
_reflns_number_gt                4290
_reflns_number_total             4666
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      1531.93
_oxford_refine_ls_r_factor_ref   0.0266
_oxford_refine_ls_scale          0.0263492(13)
_oxford_reflns_number_all        4666
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'SF_21_2_0m in R-3c'
_cod_data_source_file            ic900552b_si_002_5.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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        14152.0(7)
_cod_original_sg_symbol_Hall     '-R 3 2"c '
_cod_original_sg_symbol_H-M      'R -3 c '
_cod_original_formula_sum        'C45 H54 Co1 I1 N3 P3'
_cod_database_code               4302567
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3
-x+y,y,z+1/2
x-y,-y,-z+1/2
-x+y+1/3,y+2/3,z+7/6
x-y+1/3,-y+2/3,-z+7/6
-x+y+2/3,y+1/3,z+5/6
x-y+2/3,-y+1/3,-z+5/6
x,x-y,z+1/2
-x,-x+y,-z+1/2
x+1/3,x-y+2/3,z+7/6
-x+1/3,-x+y+2/3,-z+7/6
x+2/3,x-y+1/3,z+5/6
-x+2/3,-x+y+1/3,-z+5/6
-y,-x,z+1/2
y,x,-z+1/2
-y+1/3,-x+2/3,z+7/6
y+1/3,x+2/3,-z+7/6
-y+2/3,-x+1/3,z+5/6
y+2/3,x+1/3,-z+5/6
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
I1 I 0.6667 0.3333 0.008759(2) 0.0273 1.0000 Uani S T . . . . .
Co1 Co 0.6667 0.3333 -0.025519(4) 0.0180 1.0000 Uani S T . . . . .
P1 P 0.50560(3) 0.26316(3) -0.037599(4) 0.0202 1.0000 Uani . . . . . . .
N1 N 0.43000(9) 0.29360(10) -0.025074(16) 0.0235 1.0000 Uani . . . . . . .
C1 C 0.49087(11) 0.30301(11) -0.060162(18) 0.0234 1.0000 Uani . . . . . . .
C2 C 0.47111(11) 0.38519(12) -0.062392(19) 0.0266 1.0000 Uani . . . . . . .
C3 C 0.46821(12) 0.42123(13) -0.07960(2) 0.0325 1.0000 Uani . . . . . . .
C4 C 0.48485(13) 0.37605(13) -0.09462(2) 0.0353 1.0000 Uani . . . . . . .
C5 C 0.50581(13) 0.29547(13) -0.09256(2) 0.0337 1.0000 Uani . . . . . . .
C6 C 0.50934(12) 0.25934(12) -0.075425(19) 0.0274 1.0000 Uani . . . . . . .
C7 C 0.43442(10) 0.12060(11) -0.038973(18) 0.0234 1.0000 Uani . . . . . . .
C8 C 0.36142(12) 0.06106(12) -0.05215(2) 0.0308 1.0000 Uani . . . . . . .
C9 C 0.31116(14) -0.04672(13) -0.05156(3) 0.0396 1.0000 Uani . . . . . . .
C10 C 0.33113(13) -0.09726(13) -0.03773(3) 0.0380 1.0000 Uani . . . . . . .
C11 C 0.40206(12) -0.03957(12) -0.02442(2) 0.0315 1.0000 Uani . . . . . . .
C12 C 0.45295(11) 0.06840(11) -0.025024(19) 0.0257 1.0000 Uani . . . . . . .
C13 C 0.31728(11) 0.24996(12) -0.027507(19) 0.0264 1.0000 Uani . . . . . . .
C14 C 0.28900(13) 0.33448(14) -0.02449(2) 0.0334 1.0000 Uani . . . . . . .
C15 C 0.25356(14) 0.15708(15) -0.01517(3) 0.0403 1.0000 Uani . . . . . . .
H1 H 0.4482(17) 0.3050(17) -0.0146(3) 0.041(6) 1.0000 Uiso . . . . . . .
H21 H 0.4599 0.4167 -0.0521 0.0311 1.0000 Uiso R . . . . . .
H31 H 0.4547 0.4770 -0.0810 0.0378 1.0000 Uiso R . . . . . .
H41 H 0.4815 0.4002 -0.1063 0.0377 1.0000 Uiso R . . . . . .
H51 H 0.5182 0.2652 -0.1029 0.0376 1.0000 Uiso R . . . . . .
H61 H 0.5242 0.2044 -0.0741 0.0316 1.0000 Uiso R . . . . . .
H81 H 0.3464 0.0946 -0.0616 0.0348 1.0000 Uiso R . . . . . .
H91 H 0.2623 -0.0864 -0.0607 0.0426 1.0000 Uiso R . . . . . .
H101 H 0.2964 -0.1711 -0.0375 0.0426 1.0000 Uiso R . . . . . .
H111 H 0.4156 -0.0739 -0.0149 0.0369 1.0000 Uiso R . . . . . .
H121 H 0.5013 0.1077 -0.0158 0.0307 1.0000 Uiso R . . . . . .
H131 H 0.3008 0.2268 -0.0396 0.0326 1.0000 Uiso R . . . . . .
H141 H 0.3295 0.3915 -0.0323 0.0440 1.0000 Uiso R . . . . . .
H142 H 0.3028 0.3572 -0.0123 0.0440 1.0000 Uiso R . . . . . .
H143 H 0.2172 0.3074 -0.0270 0.0440 1.0000 Uiso R . . . . . .
H151 H 0.2723 0.1054 -0.0173 0.0489 1.0000 Uiso R . . . . . .
H152 H 0.2672 0.1789 -0.0030 0.0489 1.0000 Uiso R . . . . . .
H153 H 0.1816 0.1291 -0.0176 0.0489 1.0000 Uiso R . . . . . .
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'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 '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_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 7_655 Co1 . P1 13_665 105.296(13) yes
P1 7_655 Co1 . I1 . 113.380(11) yes
P1 13_665 Co1 . I1 . 113.380(11) yes
P1 7_655 Co1 . P1 . 105.296(13) yes
P1 13_665 Co1 . P1 . 105.296(12) yes
I1 . Co1 . P1 . 113.380(11) yes
Co1 . P1 . N1 . 110.47(4) yes
Co1 . P1 . C1 . 119.02(5) yes
N1 . P1 . C1 . 102.51(6) yes
Co1 . P1 . C7 . 114.81(5) yes
N1 . P1 . C7 . 105.27(6) yes
C1 . P1 . C7 . 103.25(6) yes
P1 . N1 . C13 . 125.25(10) yes
P1 . N1 . H1 . 112.8(15) no
C13 . N1 . H1 . 113.3(15) no
P1 . C1 . C2 . 120.13(11) yes
P1 . C1 . C6 . 120.71(11) yes
C2 . C1 . C6 . 118.86(13) yes
C1 . C2 . C3 . 120.18(14) yes
C1 . C2 . H21 . 119.9 no
C3 . C2 . H21 . 119.9 no
C2 . C3 . C4 . 120.35(15) yes
C2 . C3 . H31 . 119.8 no
C4 . C3 . H31 . 119.9 no
C3 . C4 . C5 . 119.95(14) yes
C3 . C4 . H41 . 119.9 no
C5 . C4 . H41 . 120.2 no
C4 . C5 . C6 . 120.07(15) yes
C4 . C5 . H51 . 119.9 no
C6 . C5 . H51 . 120.0 no
C1 . C6 . C5 . 120.57(15) yes
C1 . C6 . H61 . 119.6 no
C5 . C6 . H61 . 119.9 no
P1 . C7 . C8 . 125.79(11) yes
P1 . C7 . C12 . 115.94(10) yes
C8 . C7 . C12 . 118.21(13) yes
C7 . C8 . C9 . 120.44(15) yes
C7 . C8 . H81 . 119.8 no
C9 . C8 . H81 . 119.7 no
C8 . C9 . C10 . 120.62(15) yes
C8 . C9 . H91 . 119.7 no
C10 . C9 . H91 . 119.6 no
C9 . C10 . C11 . 119.74(15) yes
C9 . C10 . H101 . 120.0 no
C11 . C10 . H101 . 120.2 no
C10 . C11 . C12 . 119.77(15) yes
C10 . C11 . H111 . 120.0 no
C12 . C11 . H111 . 120.2 no
C7 . C12 . C11 . 121.20(14) yes
C7 . C12 . H121 . 119.3 no
C11 . C12 . H121 . 119.5 no
N1 . C13 . C14 . 109.85(12) yes
N1 . C13 . C15 . 112.22(12) yes
C14 . C13 . C15 . 110.70(13) yes
N1 . C13 . H131 . 107.8 no
C14 . C13 . H131 . 108.0 no
C15 . C13 . H131 . 108.1 no
C13 . C14 . H141 . 109.4 no
C13 . C14 . H142 . 109.4 no
H141 . C14 . H142 . 109.5 no
C13 . C14 . H143 . 109.5 no
H141 . C14 . H143 . 109.5 no
H142 . C14 . H143 . 109.5 no
C13 . C15 . H151 . 109.4 no
C13 . C15 . H152 . 109.6 no
H151 . C15 . H152 . 109.5 no
C13 . C15 . H153 . 109.5 no
H151 . C15 . H153 . 109.5 no
H152 . C15 . H153 . 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 . Co1 . 2.5455(3) yes
Co1 . P1 7_655 2.2605(4) yes
Co1 . P1 13_665 2.2605(4) yes
Co1 . P1 . 2.2605(4) yes
P1 . N1 . 1.6831(12) yes
P1 . C1 . 1.8259(14) yes
P1 . C7 . 1.8343(14) yes
N1 . C13 . 1.4715(18) yes
N1 . H1 . 0.81(2) no
C1 . C2 . 1.399(2) yes
C1 . C6 . 1.399(2) yes
C2 . C3 . 1.394(2) yes
C2 . H21 . 0.950 no
C3 . C4 . 1.386(2) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.386(3) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.392(2) yes
C5 . H51 . 0.950 no
C6 . H61 . 0.950 no
C7 . C8 . 1.3979(19) yes
C7 . C12 . 1.4003(19) yes
C8 . C9 . 1.386(2) yes
C8 . H81 . 0.950 no
C9 . C10 . 1.388(3) yes
C9 . H91 . 0.950 no
C10 . C11 . 1.385(2) yes
C10 . H101 . 0.950 no
C11 . C12 . 1.389(2) yes
C11 . H111 . 0.950 no
C12 . H121 . 0.950 no
C13 . C14 . 1.525(2) yes
C13 . C15 . 1.526(2) yes
C13 . H131 . 0.950 no
C14 . H141 . 0.950 no
C14 . H142 . 0.950 no
C14 . H143 . 0.950 no
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C15 . H153 . 0.950 no
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 111 2 ' '
2 0.000 1.000 0.250 209 44 ' '
3 0.000 0.000 0.500 111 2 ' '
4 0.000 0.000 0.750 209 44 ' '
5 0.333 0.667 0.417 209 44 ' '
6 0.333 0.667 0.917 209 44 ' '
7 0.333 0.667 0.167 111 2 ' '
8 0.333 0.667 0.667 111 2 ' '
9 0.667 0.333 0.083 209 44 ' '
10 0.667 0.333 0.583 209 44 ' '
11 0.667 0.333 0.333 111 2 ' '
12 0.667 0.333 0.833 111 2 ' '
