Two azido-bridged [2×2] cobalt(ii) grids featuring single-molecule magnet behaviour.
Guo, Zhilin; Deng, Yi-Fei; Zhang, Yipei; Pikramenou, Zoe; Zhang, Yuan-Zhu; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9218–9222; doi:10.1039/d0dt01461c

data_7704671
_publ_section_title
;
 Two azido-bridged [2\\times 2] cobalt(ii) grids featuring single-molecule
 magnet behaviour.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9218
_journal_page_last               9222
_journal_paper_doi               10.1039/d0dt01461c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C56 H64 Co4 N36, 3(C H Cl3), 2(C H4 O), 4(C24 H20 B), 4(C2 H3 N)'
_chemical_formula_sum            'C165 H167 B4 Cl9 Co4 N40 O2'
_chemical_formula_weight         3340.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-16 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                89.170(5)
_cell_angle_beta                 72.435(5)
_cell_angle_gamma                62.773(5)
_cell_formula_units_Z            2
_cell_length_a                   17.9901(18)
_cell_length_b                   19.0049(19)
_cell_length_c                   28.923(3)
_cell_measurement_reflns_used    9318
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.36
_cell_volume                     8293.6(15)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            197542
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         0.746
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             3468
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00046(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2104
_refine_ls_number_reflns         37633
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0427P)^2^+14.2202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30330
_reflns_number_total             37633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01461c2.cif
_cod_data_source_block           co4pzdz
_cod_depositor_comments
'Adding full bibliography for 7704671--7704672.cif.'
_cod_database_code               7704671
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.915
_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, All O(H) groups
2. Restrained distances
 Cl3A-C3AA = Cl0A-C2AA = Cl6A-C4AA = Cl7A-C4AA = Cl1A-C2AA = Cl8A-C4AA = Cl2A-
 C2AA = Cl5A-C3AA = Cl4A-C3AA
 1.79 with sigma of 0.02
 C1A-C1B = C163-C160
 1.5 with sigma of 0.02
 N38A-C1A
 1.1 with sigma of 0.02
 C160-N38
 1.1 with sigma of 0.02
 O3-C1AA
 1.42 with sigma of 0.01
 Cl6A-Cl7A = Cl0A-Cl1A = Cl3A-Cl5A
 2.88 with sigma of 0.04
 Cl3A-Cl4A = Cl0A-Cl2A = Cl8A-Cl6A
 2.88 with sigma of 0.04
 Cl4A-Cl5A = Cl2A-Cl1A = Cl8A-Cl7A
 2.88 with sigma of 0.04
 C1B-N38A
 2.56 with sigma of 0.04
 N38-C163
 2.65 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl0A \\sim C2AA \\sim Cl2A \\sim Cl1A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
N38 \\sim C160 \\sim C163: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl0A) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(Cl1A) \\sim Ueq,
Uanis(Cl2A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C0AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C161) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C163) \\sim Ueq, Uanis(C160) \\sim Ueq, Uanis(N38) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3A) = Uanis(Cl0A) = Uanis(Cl6A)
Uanis(C2AA) = Uanis(C3AA) = Uanis(C4AA)
Uanis(Cl8A) = Uanis(Cl5A)
Uanis(Cl1A) = Uanis(Cl7A)
Uanis(Cl4A) = Uanis(Cl2A)
Uanis(C163) = Uanis(C1B)
Uanis(C160) = Uanis(C1A)
Uanis(N38) = Uanis(N38A)
4. Others
 Sof(Cl5A)=Sof(Cl4A)=Sof(Cl6A)=Sof(Cl7A)=Sof(Cl3A)=Sof(Cl8A)=Sof(C4AA)=
 Sof(H4AA)=Sof(C3AA)=Sof(H3AA)=0.5*(1-FVAR(2))
 Sof(Cl0A)=Sof(Cl2A)=Sof(Cl1A)=Sof(C2AA)=Sof(H2AA)=FVAR(1)
 Sof(C1A)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(N38A)=1-FVAR(2)
 Sof(N38)=Sof(C160)=Sof(C163)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(2)
 Fixed Sof: O2(0.5) H2(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) O3(0.5)
 H3(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
5.a Ternary CH refined with riding coordinates:
 C144(H144), C162(H162), C2AA(H2AA), C4AA(H4AA), C3AA(H3AA)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28), C33(H33), C38(H38), C44(H44), C45(H45), C49(H49), C51(H51),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
 C59(H59), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70),
  C71(H71), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
 C81(H81), C82(H82), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90),
  C91(H91), C92(H92), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
 C99(H99), C100(H100), C101(H101), C102(H102), C107(H107), C108(H108),
 C111(H111), C112(H112), C114(H114), C115(H115), C116(H116), C117(H117),
 C119(H119), C120(H120), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C127(H127), C130(H130), C131(H131), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C139(H139),
 C140(H140), C141(H141), C142(H142), C143(H143), C145(H145), C146(H146),
 C147(H147), C148(H148), C149(H149), C150(H150), C153(H153), C154(H154),
 C158(H158)
5.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C73(H73A,H73B,H73C), C84(H84A,H84B,
 H84C), C93(H93A,H93B,H93C), C103(H10A,H10B,H10C), C104(H10D,H10E,H10F),
 C105(H10G,H10H,H10I), C109(H10J,H10K,H10L), C110(H11A,H11B,H11C), C113(H11D,
 H11E,H11F), C118(H11G,H11H,H11I), C121(H12A,H12B,H12C), C128(H12D,H12E,H12F),
 C129(H12G,H12H,H12I), C151(H15D,H15E,H15F), C152(H15A,H15B,H15C), C156(H15J,
 H15K,H15L), C159(H15G,H15H,H15I), C161(H16D,H16E,H16F), C163(H16A,H16B,H16C),
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3)
;
_shelx_res_checksum              52787
_olex2_submission_special_instructions 'No special instructions were received'