A metal-radical hetero-tri-spin SCM with methyl-pyrazole-nitronyl nitroxide bridges.
Huang, Xiaohui; Wang, Kang; Han, Jing; Xie, Junfang; Li, Licun; Sutter, Jean-Pascal; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11992–11998; doi:10.1039/d1dt02006d

data_7707854
_publ_section_title
;
 A metal-radical hetero-tri-spin SCM with methyl-pyrazole-nitronyl
 nitroxide bridges.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11992
_journal_page_last               11998
_journal_paper_doi               10.1039/d1dt02006d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C94 H78 Cu2 F60 N16 O28 Tb2'
_chemical_formula_sum            'C94 H78 Cu2 F60 N16 O28 Tb2'
_chemical_formula_weight         3464.64
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                112.959(3)
_cell_angle_beta                 94.439(3)
_cell_angle_gamma                107.849(3)
_cell_formula_units_Z            2
_cell_length_a                   14.5042(5)
_cell_length_b                   22.9100(8)
_cell_length_c                   25.2112(9)
_cell_measurement_reflns_used    22887
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      31.9
_cell_measurement_theta_min      1.813
_cell_volume                     7154.8(5)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.1500
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.1050
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            76660
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.578
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.5597
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       prism
_exptl_crystal_F_000             3412
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.697
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1845
_refine_ls_number_reflns         29211
_refine_ls_number_restraints     1296
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0652
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18550
_reflns_number_total             29211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02006d5.cif
_cod_data_source_block           tb-cu
_cod_depositor_comments
'Adding full bibliography for 7707852--7707854.cif.'
_cod_original_cell_volume        7154.7(5)
_cod_database_code               7707854
_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. Uiso/Uaniso restraints and constraints
C18 \\sim C25 \\sim C27 \\sim C2 \\sim C5 \\sim C78 \\sim C19 \\sim C6 \\sim
C24 \\sim C26 \\sim C17 \\sim C73 \\sim C63 \\sim C92 \\sim C4 \\sim C3 \\sim
C20 \\sim C76 \\sim C69 \\sim C93 \\sim C71 \\sim C21 \\sim C48 \\sim C58 \\sim
C31 \\sim C61 \\sim C41 \\sim C62 \\sim C14 \\sim C22 \\sim C77 \\sim C32 \\sim
C16 \\sim C79 \\sim C40 \\sim C57 \\sim C8 \\sim C13 \\sim C68 \\sim C67 \\sim
C42 \\sim C72 \\sim C49 \\sim C15 \\sim C46 \\sim C74 \\sim C53 \\sim C33 \\sim
C90 \\sim C54 \\sim C60 \\sim C23 \\sim C36 \\sim C28 \\sim C91 \\sim C88 \\sim
C50 \\sim C44 \\sim C66 \\sim C39 \\sim C11 \\sim C55 \\sim C43 \\sim C83 \\sim
C59 \\sim C51 \\sim C35 \\sim C75 \\sim C56 \\sim C81 \\sim C52 \\sim C9 \\sim
C29 \\sim C64 \\sim C86 \\sim C47 \\sim C1 \\sim C7 \\sim C80 \\sim C12 \\sim
C34 \\sim C94 \\sim C82 \\sim C38 \\sim C45 \\sim C70 \\sim C89 \\sim C30 \\sim
C87 \\sim C65 \\sim C10 \\sim C37 \\sim C84 \\sim C85: within 3.8A with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C24(H24), C26(H26), C92(H92), C4(H4), C20(H20), C62(H62), C22(H22),
 C77(H77), C42(H42), C72(H72), C44(H44), C52(H52), C47(H47), C82(H82), C87(H87)
3.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C16(H16A,H16B,H16C), C8(H8A,H8B,
 H8C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C33(H33A,H33B,H33C), C23(H23A,
 H23B,H23C), C11(H11A,H11B,H11C), C43(H43A,H43B,H43C), C35(H35A,H35B,H35C),
 C29(H29A,H29B,H29C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
 C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C30(H30A,H30B,H30C), C10(H10A,H10B,
 H10C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              94859
_shelx_hkl_checksum              44794
_shelx_fab_checksum              41107
_olex2_submission_special_instructions 'No special instructions were received'