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_7707853
_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 Dy2 F60 N16 O28'
_chemical_formula_sum            'C94 H78 Cu2 Dy2 F60 N16 O28'
_chemical_formula_weight         3471.80
_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)
;
_audit_update_record
;
????
;
_cell_angle_alpha                113.05(3)
_cell_angle_beta                 94.12(3)
_cell_angle_gamma                108.15(3)
_cell_formula_units_Z            2
_cell_length_a                   14.544(3)
_cell_length_b                   23.084(5)
_cell_length_c                   25.331(5)
_cell_measurement_reflns_used    17031
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8505
_cell_measurement_theta_min      1.4812
_cell_volume                     7251(4)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            58566
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         1.481
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.7159
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       prism
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.587
_refine_diff_density_min         -1.784
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1845
_refine_ls_number_reflns         24787
_refine_ls_number_restraints     1230
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0730
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16637
_reflns_number_total             24787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02006d3.cif
_cod_data_source_block           dy-cu
_cod_depositor_comments
'Adding full bibliography for 7707852--7707854.cif.'
_cod_original_cell_volume        7251(3)
_cod_database_code               7707853
_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
C5 \\sim C40 \\sim C4 \\sim C41 \\sim C18 \\sim C3 \\sim C68 \\sim C46 \\sim C9
\\sim C48 \\sim C51 \\sim C53 \\sim C42 \\sim C20 \\sim C87 \\sim C66 \\sim C17
\\sim C22 \\sim C6 \\sim C47 \\sim C8 \\sim C19 \\sim C36 \\sim C27 \\sim C60
\\sim C86 \\sim C1 \\sim C67 \\sim C2 \\sim C44 \\sim C26 \\sim C63 \\sim C43
\\sim C39 \\sim C15 \\sim C88 \\sim C78 \\sim C34 \\sim C57 \\sim C62 \\sim C24
\\sim C25 \\sim C83 \\sim C61 \\sim C81 \\sim C13 \\sim C76 \\sim C16 \\sim C7
\\sim C38 \\sim C45 \\sim C89 \\sim C11 \\sim C50 \\sim C56 \\sim C52 \\sim C69
\\sim C85 \\sim C49 \\sim C59 \\sim C91 \\sim C23 \\sim C55 \\sim C73 \\sim C10
\\sim C35 \\sim C84 \\sim C14 \\sim C28 \\sim C32 \\sim C33 \\sim C21 \\sim C79
\\sim C74 \\sim C65 \\sim C80 \\sim C93 \\sim C58 \\sim C77 \\sim C30 \\sim C90
\\sim C82 \\sim C64 \\sim C54 \\sim C31 \\sim C37 \\sim C72 \\sim C71 \\sim C70
\\sim C92 \\sim C75 \\sim C12 \\sim C29 \\sim C94: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C42(H42), C20(H20), C87(H87), C22(H22), C47(H47), C67(H67), C2(H2),
 C44(H44), C26(H26), C24(H24), C52(H52), C77(H77), C82(H82), C72(H72), C92(H92)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C43(H43A,H43B,H43C), C15(H15A,H15B,H15C),
 C34(H34A,H34B,H34C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C),
  C38(H38A,H38B,H38C), C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C10(H10A,H10B,
 H10C), C35(H35A,H35B,H35C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C21(H21A,
 H21B,H21C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C12(H12A,H12B,H12C),
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              29399
_shelx_hkl_checksum              5463
_shelx_fab_checksum              5234
_olex2_submission_special_instructions 'No special instructions were received'