Sophisticated Construction of Electronically Labile Materials: A Neutral, Radical-Rich, Cobalt Valence Tautomeric Triangle.
Li, Bao; Wang, Xiao-Ning; Kirchon, Angelo; Qin, Jun-Sheng; Pang, Jian-Dong; Zhuang, Gui-Lin; Zhou, Hong-Cai; Journal of the American Chemical Society 140 (2018) 14581–14585; doi:10.1021/jacs.8b09062

data_4133216
_publ_section_title
;
 Sophisticated Construction of Electronically Labile Materials: A Neutral,
 Radical-Rich, Cobalt Valence Tautomeric Triangle.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14581
_journal_page_last               14585
_journal_paper_doi               10.1021/jacs.8b09062
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C78 H82 Co3 N18 O6'
_chemical_formula_sum            'C78 H73 Co3 N18 O6'
_chemical_formula_weight         1535.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8460(9)
_cell_length_b                   50.973(4)
_cell_length_c                   15.9080(11)
_cell_measurement_reflns_used    3220
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.575
_cell_measurement_theta_min      3.468
_cell_volume                     9573.4(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_number            4872
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        50.575
_diffrn_reflns_theta_max         50.575
_diffrn_reflns_theta_min         3.468
_exptl_absorpt_coefficient_mu    4.437
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       plate
_exptl_crystal_F_000             3184
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         4872
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.339
_refine_ls_R_factor_all          0.1762
_refine_ls_R_factor_gt           0.1224
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3259
_refine_ls_wR_factor_ref         0.3560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2779
_reflns_number_total             4872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09062_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        9573.3(12)
_cod_database_code               4133216
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H30C-H41A_$2
 1.9 with sigma of 0.01
 C20-C19
 1.4 with sigma of 0.005
 N2-N3 = N4-N5
 1.4 with sigma of 0.01
 N2-C6 = N4-C6 = N3-C7 = C7-N5
 1.3 with sigma of 0.01
 N2-N4 = N3-N5
 2.4 with sigma of 0.01
 N2-N5 = N3-N4
 2.8 with sigma of 0.01
 N2-C7 = C7-N4 = C6-N3 = C6-N5
 2.25 with sigma of 0.01
 N8-N7
 1.4 with sigma of 0.01
 N8_$1-C18_$1
 1.3 with sigma of 0.01
 N8-N8_$1
 2.6 with sigma of 0.01
 C18-N7_$1
 1.3 with sigma of 0.01
 N7_$1-C18_$1
 2.4 with sigma of 0.01
 C29-C30
 1.4 with sigma of 0.01
 C33-C33_$1
 1.4 with sigma of 0.01
 C20-O2
 1.35 with sigma of 0.01
 C25-C21 \\sim C25-C26 \\sim C25-C28 \\sim C25-C27
 with sigma of 0.02
 C21-C26 \\sim C21-C28 \\sim C26-C28
 with sigma of 0.04
 C27-C21 \\sim C27-C26 \\sim C27-C28
 with sigma of 0.04
 C29-C23 \\sim C29-C31 \\sim C29-C30 \\sim C29-C32
 with sigma of 0.02
 C23-C31 \\sim C23-C30 \\sim C31-C30
 with sigma of 0.04
 C32-C23 \\sim C32-C31 \\sim C32-C30
 with sigma of 0.04
 C36-C37 \\sim C36-C39 \\sim C36-C38 \\sim C36-C34
 with sigma of 0.02
 C37-C39 \\sim C37-C38 \\sim C39-C38
 with sigma of 0.04
 C34-C37 \\sim C34-C39 \\sim C34-C38
 with sigma of 0.04
 C40-C35 \\sim C40-C43 \\sim C40-C41 \\sim C40-C42
 with sigma of 0.02
 C35-C43 \\sim C35-C41 \\sim C43-C41
 with sigma of 0.04
 C42-C35 \\sim C42-C43 \\sim C42-C41
 with sigma of 0.04
3. Restrained planarity
 C7, N5, N4, C6, N2, N3
 with sigma of 0.025
 C18, N8, N7, C18_$1, N8_$1, N7_$1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C27 \\sim C25 \\sim C21 \\sim C26 \\sim C28: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C32 \\sim C29 \\sim C23 \\sim C31 \\sim C30: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C34 \\sim C36 \\sim C37 \\sim C39 \\sim C38: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C42 \\sim C40 \\sim C35 \\sim C43 \\sim C41: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C6) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C19) = Uanis(C20)
5. Rigid body (RIGU) restrains
 C27, C25, C21, C26, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C29, C23, C31, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C36, C37, C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, C40, C35, C43, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C36(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) H39C(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) H42C(0.5) C40(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C41(0.5)
 H41A(0.5) H41B(0.5) H41C(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C13(H13), C2(H2), C11(H11), C10(H10), C12(H12), C3(H3), C1(H1),
 C16(H16), C9(H9), C15(H15), C4(H4), C14(H14), C22(H22)
7.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C39(H39A,
 H39B,H39C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C41(H41A,H41B,H41C)
;
_shelx_res_checksum              22895
_shelx_hkl_checksum              57237
_olex2_submission_special_instructions 'No special instructions were received'