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_7707852
_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 Gd2 N16 O28'
_chemical_formula_sum            'C94 H78 Cu2 F60 Gd2 N16 O28'
_chemical_formula_weight         3461.30
_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             2019-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                113.252(4)
_cell_angle_beta                 94.091(4)
_cell_angle_gamma                107.833(5)
_cell_formula_units_Z            2
_cell_length_a                   14.5495(7)
_cell_length_b                   22.9890(12)
_cell_length_c                   25.2616(10)
_cell_measurement_reflns_used    13149
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      30.8500
_cell_measurement_theta_min      1.9440
_cell_volume                     7209.5(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1574
_diffrn_reflns_av_unetI/netI     0.1605
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_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            66500
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.671
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18072
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prism
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.585
_refine_diff_density_min         -3.278
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1842
_refine_ls_number_reflns         25403
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.1009
_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^)+(0.1860P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2608
_refine_ls_wR_factor_ref         0.3165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14070
_reflns_number_total             25403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02006d4.cif
_cod_data_source_block           gd-cu
_cod_depositor_comments
'Adding full bibliography for 7707852--7707854.cif.'
_cod_original_cell_volume        7209.5(6)
_cod_database_code               7707852
_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
Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C47(H47), C42(H42), C22(H22), C87(H87), C20(H20), C44(H44), C62(H62),
 C2(H2), C52(H52), C57(H57), C67(H67), C77(H77), C26(H26), C72(H72), C24(H24),
 C92(H92)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C1(H1A,H1B,H1C), C34(H34A,H34B,H34C), C7(H7A,H7B,H7C),
 C8(H8A,H8B,H8C), C43(H43A,H43B,H43C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C),
  C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C10(H10A,H10B,H10C), C21(H21A,H21B,
 H21C), C37(H37A,H37B,H37C), C16(H16A,H16B,H16C), C29(H29A,H29B,H29C), C13(H13A,
 H13B,H13C), C33(H33A,H33B,H33C), C12(H12A,H12B,H12C), C32(H32A,H32B,H32C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              32213
_shelx_hkl_checksum              99532
_shelx_fab_checksum              5006
_olex2_submission_special_instructions 'No special instructions were received'