#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/51/4325113.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_4325113
loop_
_publ_author_name
'Vinay N. Setty'
'Wen Zhou'
'Bruce M. Foxman'
'Christine M. Thomas'
_publ_section_title
;
 Subtle Differences Between Zr and Hf in Early/Late Heterobimetallic
 Complexes with Cobalt
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4647
_journal_page_last               4655
_journal_paper_doi               10.1021/ic200445x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C45 H75 Cl1 Co1 Hf1 I1 N3 P3'
_chemical_formula_sum            'C45 H75 Cl Co Hf I N3 P3'
_chemical_formula_weight         1150.81
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-09-23
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.0541(3)
_cell_length_b                   12.0541(3)
_cell_length_c                   19.7252(7)
_cell_measurement_reflns_used    8186
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2482.11(12)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.034
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38543
_diffrn_reflns_theta_full        30.060
_diffrn_reflns_theta_max         30.060
_diffrn_reflns_theta_min         1.951
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.229
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9670
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.0032887
_refine_ls_shift/su_mean         0.0000756
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 3.38P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0446
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0446
_reflns_limit_h_max              8
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                4136
_reflns_number_total             4850
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.04
_oxford_diffrn_Wilson_scale      93.56
_oxford_refine_ls_r_factor_ref   0.0282
_oxford_refine_ls_scale          0.104819(14)
_oxford_reflns_number_all        4850
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT45_0m in P-3'
_cod_data_source_file            ic200445x_si_002_2.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P -3 '
_cod_original_formula_sum        'C45 H75 Cl1 Co1 Hf1 I1 N3 P3'
_cod_database_code               4325113
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_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
-y,x-y,z
y,-x+y,-z
-x+y,-x,z
x-y,x,-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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Hf1 Hf 0.6667 0.3333 0.726896(7) 0.0110 1.0000 Uani S T
I1 I 0.6667 0.3333 0.994719(11) 0.0203 1.0000 Uani S T
Co1 Co 0.6667 0.3333 0.86296(2) 0.0112 1.0000 Uani S T
Cl1 Cl 0.6667 0.3333 0.60537(4) 0.0203 1.0000 Uani S T
P1 P 0.63381(5) 0.49704(4) 0.82048(2) 0.0127 1.0000 Uani . .
N11 N 0.66631(15) 0.50715(15) 0.73677(8) 0.0134 1.0000 Uani . .
C1 C 0.73472(19) 0.65834(18) 0.85985(10) 0.0181 1.0000 Uani . .
C2 C 0.7111(2) 0.7642(2) 0.83283(12) 0.0268 1.0000 Uani . .
C3 C 0.7286(2) 0.6586(2) 0.93731(11) 0.0261 1.0000 Uani . .
C4 C 0.46297(18) 0.45059(19) 0.83081(10) 0.0172 1.0000 Uani . .
C5 C 0.4146(2) 0.4111(2) 0.90348(11) 0.0232 1.0000 Uani . .
C6 C 0.4204(2) 0.5419(2) 0.80261(12) 0.0272 1.0000 Uani . .
C7 C 0.6614(2) 0.58982(18) 0.68503(10) 0.0169 1.0000 Uani . .
C8 C 0.5522(2) 0.5456(2) 0.64374(10) 0.0211 1.0000 Uani . .
C9 C 0.5504(3) 0.6242(2) 0.59212(11) 0.0281 1.0000 Uani . .
C10 C 0.6537(3) 0.7442(2) 0.57901(11) 0.0302 1.0000 Uani . .
C11 C 0.7606(3) 0.7845(2) 0.61887(11) 0.0274 1.0000 Uani . .
C12 C 0.7688(2) 0.71096(19) 0.67147(11) 0.0210 1.0000 Uani . .
C13 C 0.4364(2) 0.4154(2) 0.65132(12) 0.0263 1.0000 Uani . .
C14 C 0.6499(4) 0.8250(3) 0.52182(13) 0.0443 1.0000 Uani . .
C15 C 0.8930(2) 0.7661(2) 0.70994(12) 0.0267 1.0000 Uani . .
H11 H 0.8206 0.6809 0.8481 0.0215 1.0000 Uiso . .
H21 H 0.6375 0.7600 0.8549 0.0395 1.0000 Uiso . .
H22 H 0.7851 0.8468 0.8424 0.0404 1.0000 Uiso . .
H23 H 0.6966 0.7580 0.7839 0.0390 1.0000 Uiso . .
H31 H 0.7919 0.7419 0.9527 0.0384 1.0000 Uiso . .
H32 H 0.6459 0.6446 0.9512 0.0385 1.0000 Uiso . .
H33 H 0.7452 0.5968 0.9573 0.0384 1.0000 Uiso . .
H41 H 0.4190 0.3726 0.8047 0.0213 1.0000 Uiso . .
H51 H 0.4468 0.3593 0.9234 0.0348 1.0000 Uiso . .
H52 H 0.3249 0.3619 0.9034 0.0347 1.0000 Uiso . .
H53 H 0.4377 0.4841 0.9320 0.0351 1.0000 Uiso . .
H61 H 0.3307 0.4941 0.7910 0.0404 1.0000 Uiso . .
H62 H 0.4337 0.6042 0.8350 0.0407 1.0000 Uiso . .
H63 H 0.4672 0.5848 0.7617 0.0397 1.0000 Uiso . .
H91 H 0.4772 0.5937 0.5650 0.0336 1.0000 Uiso . .
H111 H 0.8316 0.8636 0.6112 0.0327 1.0000 Uiso . .
H131 H 0.4247 0.3663 0.6120 0.0400 1.0000 Uiso . .
H132 H 0.4449 0.3691 0.6877 0.0398 1.0000 Uiso . .
H133 H 0.3608 0.4180 0.6578 0.0396 1.0000 Uiso . .
H141 H 0.6647 0.9049 0.5367 0.0671 1.0000 Uiso . .
H142 H 0.5707 0.7854 0.4982 0.0682 1.0000 Uiso . .
H143 H 0.7116 0.8398 0.4891 0.0674 1.0000 Uiso . .
H151 H 0.8951 0.7077 0.7422 0.0386 1.0000 Uiso . .
H152 H 0.9092 0.8424 0.7340 0.0404 1.0000 Uiso . .
H153 H 0.9618 0.7894 0.6796 0.0398 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'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 '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'
Hf -0.5830 6.1852 29.1440 1.8326 15.1726 9.5999 14.7586 0.2751 4.3001 72.0290
8.5815 '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
P1 5_665 Hf1 P1 3_655 83.091(14) yes
P1 5_665 Hf1 N11 3_655 114.78(4) yes
P1 3_655 Hf1 N11 3_655 35.62(4) yes
P1 5_665 Hf1 N11 5_665 35.62(4) yes
P1 3_655 Hf1 N11 5_665 102.44(4) yes
N11 3_655 Hf1 N11 5_665 119.155(14) yes
P1 5_665 Hf1 Co1 . 49.979(10) yes
P1 3_655 Hf1 Co1 . 49.979(10) yes
N11 3_655 Hf1 Co1 . 84.69(4) yes
N11 5_665 Hf1 Co1 . 84.69(4) yes
P1 5_665 Hf1 Cl1 . 130.021(10) yes
P1 3_655 Hf1 Cl1 . 130.021(10) yes
N11 3_655 Hf1 Cl1 . 95.31(4) yes
N11 5_665 Hf1 Cl1 . 95.31(4) yes
Co1 . Hf1 Cl1 . 179.995 yes
P1 5_665 Hf1 P1 . 83.091(14) yes
P1 3_655 Hf1 P1 . 83.091(14) yes
N11 3_655 Hf1 P1 . 102.44(4) yes
N11 5_665 Hf1 P1 . 114.78(4) yes
Co1 . Hf1 P1 . 49.979(10) yes
P1 5_665 Hf1 N11 . 102.44(4) yes
P1 3_655 Hf1 N11 . 114.78(4) yes
N11 3_655 Hf1 N11 . 119.155(14) yes
N11 5_665 Hf1 N11 . 119.155(13) yes
Co1 . Hf1 N11 . 84.69(4) yes
Cl1 . Hf1 P1 . 130.021(10) yes
Cl1 . Hf1 N11 . 95.31(4) yes
P1 . Hf1 N11 . 35.62(4) yes
P1 5_665 Co1 P1 3_655 108.041(16) yes
P1 5_665 Co1 I1 . 110.866(15) yes
P1 3_655 Co1 I1 . 110.866(15) yes
P1 5_665 Co1 Hf1 . 69.134(15) yes
P1 3_655 Co1 Hf1 . 69.134(15) yes
I1 . Co1 Hf1 . 179.996 yes
P1 5_665 Co1 P1 . 108.041(16) yes
P1 3_655 Co1 P1 . 108.041(16) yes
I1 . Co1 P1 . 110.866(15) yes
Hf1 . Co1 P1 . 69.134(15) yes
Hf1 . P1 Co1 . 60.887(15) yes
Hf1 . P1 N11 . 46.65(5) yes
Co1 . P1 N11 . 106.19(6) yes
Hf1 . P1 C1 . 137.74(6) yes
Co1 . P1 C1 . 115.42(7) yes
N11 . P1 C1 . 108.93(8) yes
Hf1 . P1 C4 . 112.14(7) yes
Co1 . P1 C4 . 109.55(6) yes
N11 . P1 C4 . 108.17(9) yes
C1 . P1 C4 . 108.36(9) yes
P1 . N11 Hf1 . 97.73(7) yes
P1 . N11 C7 . 130.66(13) yes
Hf1 . N11 C7 . 129.82(12) yes
P1 . C1 C2 . 115.18(15) yes
P1 . C1 C3 . 114.21(14) yes
C2 . C1 C3 . 108.40(17) yes
P1 . C1 H11 . 104.1 no
C2 . C1 H11 . 107.6 no
C3 . C1 H11 . 106.7 no
C1 . C2 H21 . 110.3 no
C1 . C2 H22 . 109.3 no
H21 . C2 H22 . 108.4 no
C1 . C2 H23 . 112.4 no
H21 . C2 H23 . 108.5 no
H22 . C2 H23 . 108.0 no
C1 . C3 H31 . 107.8 no
C1 . C3 H32 . 109.3 no
H31 . C3 H32 . 107.9 no
C1 . C3 H33 . 112.6 no
H31 . C3 H33 . 108.7 no
H32 . C3 H33 . 110.5 no
P1 . C4 C5 . 112.90(14) yes
P1 . C4 C6 . 117.59(14) yes
C5 . C4 C6 . 110.56(16) yes
P1 . C4 H41 . 102.8 no
C5 . C4 H41 . 105.0 no
C6 . C4 H41 . 106.7 no
C4 . C5 H51 . 111.6 no
C4 . C5 H52 . 109.5 no
H51 . C5 H52 . 107.5 no
C4 . C5 H53 . 111.8 no
H51 . C5 H53 . 109.2 no
H52 . C5 H53 . 107.1 no
C4 . C6 H61 . 109.6 no
C4 . C6 H62 . 110.1 no
H61 . C6 H62 . 109.4 no
C4 . C6 H63 . 111.8 no
H61 . C6 H63 . 107.4 no
H62 . C6 H63 . 108.5 no
N11 . C7 C8 . 119.99(17) yes
N11 . C7 C12 . 120.95(18) yes
C8 . C7 C12 . 118.86(18) yes
C7 . C8 C9 . 119.6(2) yes
C7 . C8 C13 . 122.97(18) yes
C9 . C8 C13 . 117.4(2) yes
C8 . C9 C10 . 122.3(2) yes
C8 . C9 H91 . 118.8 no
C10 . C9 H91 . 118.9 no
C9 . C10 C11 . 117.3(2) yes
C9 . C10 C14 . 121.0(3) yes
C11 . C10 C14 . 121.8(2) yes
C10 . C11 C12 . 123.4(2) yes
C10 . C11 H111 . 119.6 no
C12 . C11 H111 . 117.0 no
C7 . C12 C11 . 118.5(2) yes
C7 . C12 C15 . 123.83(19) yes
C11 . C12 C15 . 117.6(2) yes
C8 . C13 H131 . 110.2 no
C8 . C13 H132 . 112.0 no
H131 . C13 H132 . 106.3 no
C8 . C13 H133 . 113.0 no
H131 . C13 H133 . 107.0 no
H132 . C13 H133 . 108.0 no
C10 . C14 H141 . 112.2 no
C10 . C14 H142 . 113.0 no
H141 . C14 H142 . 107.4 no
C10 . C14 H143 . 111.3 no
H141 . C14 H143 . 107.3 no
H142 . C14 H143 . 105.2 no
C12 . C15 H151 . 113.4 no
C12 . C15 H152 . 110.6 no
H151 . C15 H152 . 107.9 no
C12 . C15 H153 . 110.1 no
H151 . C15 H153 . 107.3 no
H152 . C15 H153 . 107.3 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
Hf1 P1 5_665 2.8705(5) yes
Hf1 P1 3_655 2.8705(5) yes
Hf1 N11 3_655 2.1064(15) yes
Hf1 N11 5_665 2.1064(15) yes
Hf1 Co1 . 2.6839(5) yes
Hf1 Cl1 . 2.3972(9) yes
Hf1 P1 . 2.8705(5) yes
Hf1 N11 . 2.1064(15) yes
I1 Co1 . 2.5989(5) yes
Co1 P1 5_665 2.3526(5) yes
Co1 P1 3_655 2.3526(5) yes
Co1 P1 . 2.3526(5) yes
P1 N11 . 1.6873(16) yes
P1 C1 . 1.870(2) yes
P1 C4 . 1.855(2) yes
N11 C7 . 1.448(2) yes
C1 C2 . 1.535(3) yes
C1 C3 . 1.530(3) yes
C1 H11 . 0.958 no
C2 H21 . 0.967 no
C2 H22 . 0.967 no
C2 H23 . 0.978 no
C3 H31 . 0.957 no
C3 H32 . 0.963 no
C3 H33 . 0.950 no
C4 C5 . 1.531(3) yes
C4 C6 . 1.532(3) yes
C4 H41 . 0.965 no
C5 H51 . 0.968 no
C5 H52 . 0.938 no
C5 H53 . 0.961 no
C6 H61 . 0.965 no
C6 H62 . 0.937 no
C6 H63 . 0.973 no
C7 C8 . 1.407(3) yes
C7 C12 . 1.410(3) yes
C8 C9 . 1.398(3) yes
C8 C13 . 1.498(3) yes
C9 C10 . 1.382(4) yes
C9 H91 . 0.935 no
C10 C11 . 1.374(4) yes
C10 C14 . 1.506(3) yes
C11 C12 . 1.400(3) yes
C11 H111 . 0.921 no
C12 C15 . 1.505(3) yes
C13 H131 . 0.942 no
C13 H132 . 0.945 no
C13 H133 . 0.937 no
C14 H141 . 0.934 no
C14 H142 . 0.949 no
C14 H143 . 0.933 no
C15 H151 . 0.959 no
C15 H152 . 0.964 no
C15 H153 . 0.945 no
