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#$Date: 2016-03-22 12:41:31 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178959 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/88/4118842.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_4118842
loop_
_publ_author_name
'Evan R. King'
'Graham T. Sazama'
'Theodore A. Betley'
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
Mallinckrodt 306E
12 Oxford Street
Cambridge, MA 02139
;
_publ_contact_author_email       betley@chemistry.harvard.edu
_publ_contact_author_name        'Professor Theodore A. Betley'
_publ_contact_author_phone       617-496-9944
_publ_section_title
;
 Co(III) Imidos Exhibiting Spin Crossover and C-H Bond Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17858
_journal_page_last               17861
_journal_paper_doi               10.1021/ja307699u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C71 H54 Co N3'
_chemical_formula_sum            'C71 H54 Co N3'
_chemical_formula_weight         1008.10
_chemical_name_common            (ArDpme)Co(py)
_chemical_name_systematic
; 
5-mesityl-1,9-bis(2,4,6-triphenylphenyl)dipyrrinatocobalt(I) pyridine
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.802(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.485(2)
_cell_length_b                   17.5727(17)
_cell_length_c                   14.6905(15)
_cell_measurement_reflns_used    6205
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6114
_cell_measurement_theta_min      2.3180
_cell_volume                     5269.7(9)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 goniometer with CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44229
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2009)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.623
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1234P)²+33.5892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2461
_reflns_number_gt                4374
_reflns_number_total             6045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307699u_si_002_2.cif
_cod_data_source_block           ArDpmeCoPy
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4118842
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Co1 Co 0.5000 0.21737(5) 0.2500 0.0293(3) Uani 1 2 d S
N1 N 0.55818(13) 0.29214(15) 0.31398(19) 0.0128(6) Uani 1 1 d .
N2 N 0.5000 0.1069(2) 0.2500 0.0188(9) Uani 1 2 d S
C1 C 0.61155(16) 0.28233(19) 0.3708(2) 0.0142(7) Uani 1 1 d .
C2 C 0.64094(17) 0.3528(2) 0.3986(3) 0.0187(7) Uani 1 1 d .
H2 H 0.6797 0.3598 0.4380 0.022 Uiso 1 1 calc R
C3 C 0.60240(17) 0.4086(2) 0.3575(2) 0.0174(7) Uani 1 1 d .
H3 H 0.6089 0.4620 0.3630 0.021 Uiso 1 1 calc R
C4 C 0.55037(16) 0.37083(18) 0.3045(2) 0.0146(7) Uani 1 1 d .
C5 C 0.5000 0.4064(3) 0.2500 0.0144(9) Uani 1 2 d S
C6 C 0.5564(2) 0.0670(2) 0.2562(3) 0.0272(9) Uani 1 1 d .
H6 H 0.5966 0.0941 0.2608 0.033 Uiso 1 1 calc R
C7 C 0.5580(3) -0.0117(3) 0.2561(4) 0.0510(15) Uani 1 1 d .
H7 H 0.5986 -0.0381 0.2603 0.061 Uiso 1 1 calc R
C8 C 0.5000 -0.0509(4) 0.2500 0.069(3) Uani 1 2 d S
H8 H 0.5000 -0.1050 0.2500 0.083 Uiso 1 2 calc SR
C9 C 0.63551(16) 0.20700(19) 0.4031(2) 0.0134(6) Uani 1 1 d .
C10 C 0.69922(16) 0.18469(19) 0.3840(2) 0.0147(7) Uani 1 1 d .
C11 C 0.72651(16) 0.11816(19) 0.4232(2) 0.0149(7) Uani 1 1 d .
H11 H 0.7691 0.1030 0.4093 0.018 Uiso 1 1 calc R
C12 C 0.69288(16) 0.07394(19) 0.4817(2) 0.0145(7) Uani 1 1 d .
C13 C 0.62855(16) 0.09425(19) 0.4962(2) 0.0155(7) Uani 1 1 d .
H13 H 0.6041 0.0626 0.5333 0.019 Uiso 1 1 calc R
C14 C 0.59911(16) 0.15992(19) 0.4575(2) 0.0143(7) Uani 1 1 d .
C15 C 0.73765(17) 0.23157(19) 0.3237(2) 0.0162(7) Uani 1 1 d .
C16 C 0.7113(2) 0.2523(2) 0.2362(3) 0.0227(8) Uani 1 1 d .
H16 H 0.6685 0.2362 0.2146 0.027 Uiso 1 1 calc R
C17 C 0.7485(2) 0.2970(2) 0.1805(3) 0.0301(9) Uani 1 1 d .
H17 H 0.7309 0.3107 0.1209 0.036 Uiso 1 1 calc R
C18 C 0.8102(2) 0.3210(2) 0.2115(3) 0.0319(10) Uani 1 1 d .
H18 H 0.8350 0.3512 0.1734 0.038 Uiso 1 1 calc R
C19 C 0.8361(2) 0.3014(2) 0.2980(3) 0.0290(9) Uani 1 1 d .
H19 H 0.8784 0.3189 0.3197 0.035 Uiso 1 1 calc R
C20 C 0.80035(19) 0.2559(2) 0.3538(3) 0.0224(8) Uani 1 1 d .
H20 H 0.8190 0.2414 0.4127 0.027 Uiso 1 1 calc R
C21 C 0.72658(16) 0.00985(19) 0.5321(3) 0.0160(7) Uani 1 1 d .
C22 C 0.76736(18) -0.0394(2) 0.4894(3) 0.0215(8) Uani 1 1 d .
H22 H 0.7716 -0.0346 0.4257 0.026 Uiso 1 1 calc R
C23 C 0.8021(2) -0.0958(2) 0.5396(3) 0.0292(9) Uani 1 1 d .
H23 H 0.8303 -0.1287 0.5098 0.035 Uiso 1 1 calc R
C24 C 0.7961(2) -0.1044(2) 0.6317(3) 0.0313(10) Uani 1 1 d .
H24 H 0.8200 -0.1430 0.6653 0.038 Uiso 1 1 calc R
C25 C 0.7554(2) -0.0566(2) 0.6745(3) 0.0315(9) Uani 1 1 d .
H25 H 0.7506 -0.0628 0.7378 0.038 Uiso 1 1 calc R
C26 C 0.7209(2) 0.0011(2) 0.6254(3) 0.0245(8) Uani 1 1 d .
H26 H 0.6934 0.0345 0.6559 0.029 Uiso 1 1 calc R
C27 C 0.53051(17) 0.1775(2) 0.4768(2) 0.0170(7) Uani 1 1 d .
C28 C 0.51150(18) 0.2507(2) 0.5001(3) 0.0215(8) Uani 1 1 d .
H28 H 0.5431 0.2903 0.5051 0.026 Uiso 1 1 calc R
C29 C 0.4468(2) 0.2665(2) 0.5161(3) 0.0291(9) Uani 1 1 d .
H29 H 0.4347 0.3164 0.5329 0.035 Uiso 1 1 calc R
C30 C 0.39988(19) 0.2091(3) 0.5075(3) 0.0296(9) Uani 1 1 d .
H30 H 0.3554 0.2201 0.5163 0.036 Uiso 1 1 calc R
C31 C 0.41818(19) 0.1360(3) 0.4862(3) 0.0284(9) Uani 1 1 d .
H31 H 0.3864 0.0965 0.4816 0.034 Uiso 1 1 calc R
C32 C 0.48325(18) 0.1201(2) 0.4714(3) 0.0229(8) Uani 1 1 d .
H32 H 0.4955 0.0696 0.4575 0.027 Uiso 1 1 calc R
C33 C 0.5000 0.4913(3) 0.2500 0.0155(9) Uani 1 2 d S
C34 C 0.46158(18) 0.5311(2) 0.3088(3) 0.0216(8) Uani 1 1 d .
C35 C 0.4619(2) 0.6103(2) 0.3066(3) 0.0264(9) Uani 1 1 d .
H35 H 0.4351 0.6375 0.3451 0.032 Uiso 1 1 calc R
C36 C 0.5000 0.6506(3) 0.2500 0.0266(12) Uani 1 2 d S
C37 C 0.4205(2) 0.4901(2) 0.3732(3) 0.0369(11) Uani 1 1 d .
H37A H 0.4022 0.5269 0.4142 0.055 Uiso 1 1 calc R
H37B H 0.4477 0.4533 0.4092 0.055 Uiso 1 1 calc R
H37C H 0.3848 0.4633 0.3381 0.055 Uiso 1 1 calc R
C38 C 0.5000 0.7363(3) 0.2500 0.0393(16) Uani 1 2 d S
H38A H 0.5414 0.7549 0.2803 0.059 Uiso 0.50 1 calc PR
H38B H 0.4634 0.7549 0.2828 0.059 Uiso 0.50 1 calc PR
H38C H 0.4952 0.7549 0.1869 0.059 Uiso 0.50 1 calc PR
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'
Co Co 0.3494 0.9721 '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'
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
N2 Co1 N1 132.09(8) . 2_655
N2 Co1 N1 132.09(8) . .
N1 Co1 N1 95.82(16) 2_655 .
C1 N1 C4 105.8(3) . .
C1 N1 Co1 130.4(2) . .
C4 N1 Co1 123.8(2) . .
C6 N2 C6 117.4(5) 2_655 .
C6 N2 Co1 121.3(2) 2_655 .
C6 N2 Co1 121.3(2) . .
N1 C1 C2 111.9(3) . .
N1 C1 C9 123.5(3) . .
C2 C1 C9 124.6(3) . .
C3 C2 C1 106.4(3) . .
C3 C2 H2 126.8 . .
C1 C2 H2 126.8 . .
C2 C3 C4 106.5(3) . .
C2 C3 H3 126.8 . .
C4 C3 H3 126.8 . .
N1 C4 C5 124.9(3) . .
N1 C4 C3 109.4(3) . .
C5 C4 C3 125.7(3) . .
C4 C5 C4 126.9(4) . 2_655
C4 C5 C33 116.5(2) . .
C4 C5 C33 116.5(2) 2_655 .
N2 C6 C7 122.7(4) . .
N2 C6 H6 118.6 . .
C7 C6 H6 118.6 . .
C8 C7 C6 118.8(5) . .
C8 C7 H7 120.6 . .
C6 C7 H7 120.6 . .
C7 C8 C7 119.7(6) 2_655 .
C7 C8 H8 120.2 2_655 .
C7 C8 H8 120.2 . .
C14 C9 C10 119.4(3) . .
C14 C9 C1 122.2(3) . .
C10 C9 C1 118.2(3) . .
C11 C10 C9 119.6(3) . .
C11 C10 C15 119.8(3) . .
C9 C10 C15 120.6(3) . .
C12 C11 C10 121.5(3) . .
C12 C11 H11 119.3 . .
C10 C11 H11 119.3 . .
C11 C12 C13 118.4(3) . .
C11 C12 C21 120.0(3) . .
C13 C12 C21 121.5(3) . .
C12 C13 C14 121.9(3) . .
C12 C13 H13 119.1 . .
C14 C13 H13 119.1 . .
C13 C14 C9 119.0(3) . .
C13 C14 C27 118.4(3) . .
C9 C14 C27 122.6(3) . .
C20 C15 C16 119.2(3) . .
C20 C15 C10 120.1(3) . .
C16 C15 C10 120.7(3) . .
C15 C16 C17 119.6(4) . .
C15 C16 H16 120.2 . .
C17 C16 H16 120.2 . .
C18 C17 C16 120.6(4) . .
C18 C17 H17 119.7 . .
C16 C17 H17 119.7 . .
C17 C18 C19 120.1(4) . .
C17 C18 H18 120.0 . .
C19 C18 H18 120.0 . .
C18 C19 C20 120.3(4) . .
C18 C19 H19 119.9 . .
C20 C19 H19 119.9 . .
C15 C20 C19 120.3(4) . .
C15 C20 H20 119.8 . .
C19 C20 H20 119.8 . .
C22 C21 C26 118.7(3) . .
C22 C21 C12 121.2(3) . .
C26 C21 C12 120.0(3) . .
C21 C22 C23 120.2(4) . .
C21 C22 H22 119.9 . .
C23 C22 H22 119.9 . .
C24 C23 C22 121.0(4) . .
C24 C23 H23 119.5 . .
C22 C23 H23 119.5 . .
C25 C24 C23 119.4(4) . .
C25 C24 H24 120.3 . .
C23 C24 H24 120.3 . .
C24 C25 C26 120.5(4) . .
C24 C25 H25 119.8 . .
C26 C25 H25 119.8 . .
C21 C26 C25 120.3(4) . .
C21 C26 H26 119.8 . .
C25 C26 H26 119.8 . .
C28 C27 C32 118.3(3) . .
C28 C27 C14 121.7(3) . .
C32 C27 C14 120.0(3) . .
C29 C28 C27 121.0(4) . .
C29 C28 H28 119.5 . .
C27 C28 H28 119.5 . .
C30 C29 C28 120.0(4) . .
C30 C29 H29 120.0 . .
C28 C29 H29 120.0 . .
C31 C30 C29 119.7(4) . .
C31 C30 H30 120.1 . .
C29 C30 H30 120.1 . .
C30 C31 C32 120.2(4) . .
C30 C31 H31 119.9 . .
C32 C31 H31 119.9 . .
C27 C32 C31 120.8(4) . .
C27 C32 H32 119.6 . .
C31 C32 H32 119.6 . .
C34 C33 C34 120.2(4) . 2_655
C34 C33 C5 119.9(2) . .
C34 C33 C5 119.9(2) 2_655 .
C35 C34 C33 118.7(4) . .
C35 C34 C37 119.9(3) . .
C33 C34 C37 121.4(3) . .
C36 C35 C34 122.0(4) . .
C36 C35 H35 119.0 . .
C34 C35 H35 119.0 . .
C35 C36 C35 118.4(5) 2_655 .
C35 C36 C38 120.8(2) 2_655 .
C35 C36 C38 120.8(2) . .
C34 C37 H37A 109.5 . .
C34 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
C34 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
C36 C38 H38A 109.5 . .
C36 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
C36 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.942(4) .
Co1 N1 1.960(3) 2_655
Co1 N1 1.960(3) .
N1 C1 1.330(4) .
N1 C4 1.397(4) .
N2 C6 1.346(5) 2_655
N2 C6 1.346(5) .
C1 C2 1.422(5) .
C1 C9 1.476(4) .
C2 C3 1.367(5) .
C2 H2 0.9500 .
C3 C4 1.430(5) .
C3 H3 0.9500 .
C4 C5 1.400(4) .
C5 C4 1.400(4) 2_655
C5 C33 1.492(6) .
C6 C7 1.384(6) .
C6 H6 0.9500 .
C7 C8 1.370(7) .
C7 H7 0.9500 .
C8 C7 1.370(7) 2_655
C8 H8 0.9500 .
C9 C14 1.407(5) .
C9 C10 1.413(5) .
C10 C11 1.399(5) .
C10 C15 1.484(5) .
C11 C12 1.385(5) .
C11 H11 0.9500 .
C12 C13 1.399(5) .
C12 C21 1.486(5) .
C13 C14 1.400(5) .
C13 H13 0.9500 .
C14 C27 1.489(5) .
C15 C20 1.390(5) .
C15 C16 1.400(5) .
C16 C17 1.403(6) .
C16 H16 0.9500 .
C17 C18 1.373(7) .
C17 H17 0.9500 .
C18 C19 1.379(7) .
C18 H18 0.9500 .
C19 C20 1.396(5) .
C19 H19 0.9500 .
C20 H20 0.9500 .
C21 C22 1.389(5) .
C21 C26 1.394(5) .
C22 C23 1.395(5) .
C22 H22 0.9500 .
C23 C24 1.377(7) .
C23 H23 0.9500 .
C24 C25 1.372(7) .
C24 H24 0.9500 .
C25 C26 1.402(5) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C27 C28 1.394(5) .
C27 C32 1.396(5) .
C28 C29 1.393(5) .
C28 H28 0.9500 .
C29 C30 1.391(6) .
C29 H29 0.9500 .
C30 C31 1.381(6) .
C30 H30 0.9500 .
C31 C32 1.397(5) .
C31 H31 0.9500 .
C32 H32 0.9500 .
C33 C34 1.403(4) .
C33 C34 1.403(4) 2_655
C34 C35 1.392(5) .
C34 C37 1.502(6) .
C35 C36 1.381(5) .
C35 H35 0.9500 .
C36 C35 1.381(5) 2_655
C36 C38 1.506(7) .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C38 H38A 0.9800 .
C38 H38B 0.9800 .
C38 H38C 0.9800 .
