Electronic Structure Description of a Doubly Oxidized Bimetallic Cobalt Complex with Proradical Ligands.
Clarke, Ryan M.; Hazin, Khatera; Thompson, John R.; Savard, Didier; Prosser, Kathleen E.; Storr, Tim; Inorganic chemistry 55 (2016) 762–774; doi:10.1021/acs.inorgchem.5b02231

data_4344548
_publ_section_title
;
 Electronic Structure Description of a Doubly Oxidized Bimetallic Cobalt
 Complex with Proradical Ligands.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              762
_journal_page_last               774
_journal_paper_doi               10.1021/acs.inorgchem.5b02231
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C68 H90 Co2 N4 O4'
_chemical_formula_sum            'C68 H90 Co2 N4 O4'
_chemical_formula_weight         1145.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                97.903(4)
_cell_angle_beta                 106.447(3)
_cell_angle_gamma                103.449(3)
_cell_formula_units_Z            4
_cell_length_a                   16.0869(13)
_cell_length_b                   19.859(2)
_cell_length_c                   25.845(3)
_cell_measurement_reflns_used    3475
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      22.041
_cell_measurement_theta_min      2.403
_cell_volume                     7516.5(13)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker X8 APEX 2 area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -0
_diffrn_reflns_number            17545
_diffrn_reflns_theta_full        22.475
_diffrn_reflns_theta_max         22.475
_diffrn_reflns_theta_min         1.377
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2008/2 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0624 before and 0.0496 after correction.
 The Ratio of minimum to maximum transmission is 0.74.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0699 before and 0.0525 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 52658 reflections, Rint = 0.1153
 (11901 with I > 3sig(I), Rint = 0.0497)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.414
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1493
_refine_ls_number_reflns         17545
_refine_ls_number_restraints     1488
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.1811
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.2055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8311
_reflns_number_total             17545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02231_si_002.cif
_cod_data_source_block           Co2L2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        7516.5(14)
_cod_database_code               4344548
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5732(16) 0.4268(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C61-C62 \\sim C61-C63 \\sim C61-C64
 with sigma of 0.01
 C62-C63 \\sim C63-C64 \\sim C64-C62
 with sigma of 0.01
 C61A-C62A \\sim C61A-C63A \\sim C61A-C64A
 with sigma of 0.01
 C62A-C63A \\sim C63A-C64A \\sim C64A-C62A
 with sigma of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C61A)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C64A)=Sof(H64D)=
 Sof(H64E)=Sof(H64F)=Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(1)
 Sof(C61)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=Sof(H63A)=Sof(H63B)=
 Sof(H63C)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C52(H52A,H52B), C89(H89A,H89B), C120(H12A,H12B)
6.b Me refined with riding coordinates:
 C63A(H63D,H63E,H63F)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C17(H17), C25(H25),
 C27(H27), C39(H39), C43(H43), C48(H48), C56(H56), C58(H58), C70(H70), C71(H71),
  C72(H72), C73(H73), C76(H76), C80(H80), C85(H85), C93(H93), C95(H95),
 C107(H107), C111(H111), C116(H116), C124(H124), C126(H126)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C91(H91A,
 H91B,H91C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F),
 C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C105(H10M,H10N,H10O), C113(H11A,
 H11B,H11C), C114(H11D,H11E,H11F), C115(H11G,H11H,H11I), C118(H11J,H11K,H11L),
 C119(H11M,H11N,H11O), C122(H12C,H12D,H12E), C130(H13A,H13B,H13C), C131(H13D,
 H13E,H13F), C132(H13G,H13H,H13I), C134(H13J,H13K,H13L), C135(H13M,H13N,H13O),
 C136(H13P,H13Q,H13R), C64A(H64D,H64E,H64F), C62A(H62D,H62E,H62F)
;
_shelx_res_checksum              59679
_shelx_hkl_checksum              49122
_shelx_fab_checksum              75316
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'