The ferromagnetic [Ln2Co6] heterometallic complexes.
Zhao, Xiao-Qing; Wang, Jin; Bao, Dong-Xu; Xiang, Shuo; Liu, Ya-Jun; Li, Yun-Chun; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2196–2203; doi:10.1039/c6dt04375e

data_7041675
_publ_section_title
;
 The ferromagnetic [Ln2Co6] heterometallic complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2196
_journal_page_last               2203
_journal_paper_doi               10.1039/c6dt04375e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C74 H100 Cl6 Co6 Ho2 N8 O26, C H2 Cl2'
_chemical_formula_sum            'C75 H102 Cl8 Co6 Ho2 N8 O26'
_chemical_formula_weight         2498.68
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2017-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                112.470(3)
_cell_angle_beta                 101.631(2)
_cell_angle_gamma                109.979(3)
_cell_formula_units_Z            1
_cell_length_a                   14.0733(4)
_cell_length_b                   14.5350(5)
_cell_length_c                   15.5037(5)
_cell_measurement_reflns_used    12974
_cell_measurement_temperature    121.9(2)
_cell_measurement_theta_max      29.1480
_cell_measurement_theta_min      3.3610
_cell_volume                     2544.77(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      121.9(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.6531
_diffrn_measurement_details
;
  1 omega   -7.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   77.0000 -120.0000 69

  2 omega    5.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   57.0000 -120.0000 28

  3 omega  -19.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000  -30.0000 79

  4 omega   55.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  178.0000 -150.0000 27

  5 omega   35.00   61.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497 -178.0000  120.0000 26

  6 omega  -12.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   77.0000  120.0000 97

  7 omega  -34.00   -3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5841   57.0000   30.0000 31

  8 omega    1.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5841   57.0000 -180.0000 48

  9 omega  -86.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5841  -19.0000    0.0000 89
;
_diffrn_measurement_device_type  SuperNova
_diffrn_orient_matrix_UB_11      -0.0557999000
_diffrn_orient_matrix_UB_12      -0.0402337000
_diffrn_orient_matrix_UB_13      -0.0205189000
_diffrn_orient_matrix_UB_21      0.0147992000
_diffrn_orient_matrix_UB_22      -0.0439195000
_diffrn_orient_matrix_UB_23      -0.0160258000
_diffrn_orient_matrix_UB_31      0.0060191000
_diffrn_orient_matrix_UB_32      0.0007418000
_diffrn_orient_matrix_UB_33      0.0468340000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22147
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         8963
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+11.4144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8042
_reflns_number_total             8963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04375e2.cif
_cod_data_source_block           p150407k
_cod_depositor_comments
'Adding full bibliography for 7041675--7041678.cif.'
_cod_original_cell_volume        2544.77(16)
_cod_database_code               7041675
_chemical_oxdiff_formula         C1H1O1N1CO1HO1
_chemical_oxdiff_usercomment     378
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20-C17
 1.52 with sigma of 0.02
 C20-C17A
 1.52 with sigma of 0.02
 C20-C18
 1.52 with sigma of 0.02
 C20-C18A
 1.52 with sigma of 0.02
 C20-C19
 1.52 with sigma of 0.02
 C20-C19A
 1.52 with sigma of 0.02
 C16-C17
 2.51 with sigma of 0.02
 C16-C17A
 2.51 with sigma of 0.02
 C16-C18
 2.51 with sigma of 0.02
 C16-C18A
 2.51 with sigma of 0.02
 C16-C19
 2.51 with sigma of 0.02
 C16-C19A
 2.51 with sigma of 0.02
 C17-C18
 2.51 with sigma of 0.02
 C17-C19
 2.51 with sigma of 0.02
 C18-C19
 2.51 with sigma of 0.02
 C17A-C18A
 2.51 with sigma of 0.02
 C17A-C19A
 2.51 with sigma of 0.02
 C18A-C19A
 2.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(Cl5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C17A) \\sim Ueq, Uanis(C19A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C18A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C17) = Uanis(C17A) = Uanis(C18) = Uanis(C18A) = Uanis(C19) = Uanis(C19A)
4. Others
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(3)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(3)
 Fixed Sof: Cl4(0.5) Cl5(0.5) C38(0.5) H38A(0.5) H38B(0.5) C25B(0.5) H25A(0.5)
 H25B(0.5) H25C(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5)
5.a Riding coordinates:
 O1(H1), O2(H2A)
5.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14)
5.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F),
 C25B(H25A,H25B,H25C), C1B(H1BA,H1BB,H1BC), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C17(H17A,H17B,H17C), C18A(H18D,H18E,H18F), C17A(H17D,H17E,H17F),
 C19A(H19D,H19E,H19F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'