A mononuclear transition metal single-molecule magnet in a nuclear spin-free ligand environment.
Fataftah, Majed S.; Zadrozny, Joseph M.; Rogers, Dylan M.; Freedman, Danna E.; Inorganic chemistry 53 (2014) 10716–10721; doi:10.1021/ic501906z

data_4341097
_publ_section_title
;
 A mononuclear transition metal single-molecule magnet in a nuclear
 spin-free ligand environment.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10716
_journal_page_last               10721
_journal_paper_doi               10.1021/ic501906z
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C6 Co S10, 2(C24 H20 P), C2 H3 N'
_chemical_formula_sum            'C56 H43 Co N P2 S10'
_chemical_formula_weight         1171.38
_chemical_name_systematic        Cobalt(C3S5)2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                64.432(3)
_cell_angle_beta                 78.376(3)
_cell_angle_gamma                78.050(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5256(5)
_cell_length_b                   16.9629(9)
_cell_length_c                   19.2150(10)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.116
_cell_measurement_theta_min      2.687
_cell_volume                     2717.9(3)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      99.74
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17431
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.24
_diffrn_reflns_theta_min         1.38
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0789 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.8794.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1206
_exptl_crystal_preparation
'Synthesized from addition of CoCl2 to Na2C3S5 in 10 mL of methanol.'
_exptl_crystal_recrystallization_method
'Recrystallized from hot acetonitrile.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                7585
_reflns_number_total             10408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501906z_si_002.cif
_cod_data_source_block           msf1_51_0m
_cod_depositor_comments
'Adding full bibliography for 4341097--4341098.cif.'
_cod_original_cell_volume        2717.9(2)
_cod_database_code               4341097
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
2.b Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC)
;