A mixed-valence metallogrid [CoCo] with an unusual electronic structure and single-ion-magnet characterization.
Huang, Wei; Pan, Feifei; Wang, Zhenxing; Bai, Yan; Feng, Xuejun; Gu, Jiande; Ouyang, Zhong-Wen; Wu, Dayu; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5069–5075; doi:10.1039/c7dt00564d

data_7042520
_publ_section_title
;
 A mixed-valence metallogrid [CoCo] with an unusual electronic structure
 and single-ion-magnet characterization.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5069
_journal_page_last               5075
_journal_paper_doi               10.1039/c7dt00564d
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C74 H58 Co4 N12 O14, C4 H10 O'
_chemical_formula_sum            'C78 H68 Co4 N12 O15'
_chemical_formula_weight         1649.16
_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   mixed
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.11.07 svn.r3349 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-11-18 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                74.232(2)
_cell_angle_beta                 82.418(2)
_cell_angle_gamma                66.125(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9882(11)
_cell_length_b                   15.0573(12)
_cell_length_c                   17.6800(13)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.9085
_cell_measurement_theta_min      2.4320
_cell_volume                     3510.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20076
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.197
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         12310
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1611P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.2443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8685
_reflns_number_total             12310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00564d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7042520.cif.'
_cod_database_code               7042520
_olex2_refinement_description
;
1. 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, All O(H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 O14-H14A
 0.85 with sigma of 0.01
 C73-H9
 1.852435 with sigma of 0.02
 Co4-H9
 2.449011 with sigma of 0.02
 C74-H14A
 1.900743 with sigma of 0.02
 Co2-H14A
 2.680448 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O1E, C04, C01, H04A, H04B, C03, C02
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C04(H04A,H04B), C01(H01A,H01B)
4.b Me refined with riding coordinates:
 C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C74(H74A,H74B,
 H74C), C03(H03A,H03B,H03C), C02(H02A,H02B,H02C)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C0AA(H0AA), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C25(H25), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C59(H59),
 C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C8(H8)
;
_shelx_res_checksum              44154
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'