Two-Coordinate Co(II) Imido Complexes as Outstanding Single-Molecule Magnets.
Yao, Xiao-Nan; Du, Jing-Zhen; Zhang, Yi-Quan; Leng, Xue-Bing; Yang, Mu-Wen; Jiang, Shang-Da; Wang, Zhen-Xing; Ouyang, Zhong-Wen; Deng, Liang; Wang, Bing-Wu; Gao, Song; Journal of the American Chemical Society 139 (2017) 373–380; doi:10.1021/jacs.6b11043

data_4125333
_publ_section_title
;
 Two-Coordinate Co(II) Imido Complexes as Outstanding Single-Molecule
 Magnets.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              373
_journal_page_last               380
_journal_paper_doi               10.1021/jacs.6b11043
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '2(C27.5 H33.5 Co0.5 N1.5)'
_chemical_formula_sum            'C55 H67 Co N3'
_chemical_formula_weight         829.04
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.911(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2364(13)
_cell_length_b                   16.4272(17)
_cell_length_c                   24.439(3)
_cell_measurement_reflns_used    3477
_cell_measurement_temperature    130
_cell_measurement_theta_max      21.10
_cell_measurement_theta_min      2.29
_cell_volume                     4894.4(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40285
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         0.836
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0694 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.8354.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         11675
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6027
_reflns_number_total             11675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11043_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4125333--4125335.cif.'
_cod_database_code               4125333
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.926
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C38-C39 = C4-C5 = C4-C5' = C37-C38
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C5': within 1.7A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67: within 1.7A
with sigma of 0.005 and sigma for terminal atoms of 0.01
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55: within 1.7A
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C55) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C67) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H37A(0.5) H37B(0.5) H38A(0.5) H38B(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) H40A(0.5) H40B(0.5) H4AA(0.5) H4AB(0.5) H4BC(0.5) H4BD(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) C5'(0.5) H5'A(0.5) H5'B(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5)
5.a Riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
5.b Ternary CH refined with riding coordinates:
 C46(H46), C53(H53), C12(H12), C15(H15)
5.c Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C5'(H5'A,H5'B)
5.d Aromatic/amide H refined with riding coordinates:
 C44(H44), C45(H45), C51(H51), C52(H52), C58(H58), C59(H59), C62(H62),
 C64(H64), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C26(H26),
 C32(H32)
5.e Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              95670
_shelx_hkl_checksum              22166
_olex2_submission_special_instructions 'No special instructions were received'