Slow Spin Relaxation in a Low-Spin S=1/2 FeIII Carborane Complex
Buades, Anna B.; Arderiu, Víctor S.; Maxwell, Lindley; Amoza-Davila, Martin; Choquesillo-Lazarte, Duane; Aliaga-Alcalde, Núria; Vinas, Clara; Teixidor, Francesc; Ruiz, Eliseo; Chemical Communications  (2019) –; doi:10.1039/C9CC01123D

data_7123083
_publ_section_title
;
 Slow Spin Relaxation in a Low-Spin S=1/2 FeIII Carborane Complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01123D
_journal_year                    2019
_chemical_formula_moiety         'C4 H22 B18 Fe, C4 H12 N'
_chemical_formula_sum            'C8 H34 B18 Fe N'
_chemical_formula_weight         394.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-13 deposited with the CCDC.    2019-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8764(3)
_cell_length_b                   28.8263(15)
_cell_length_c                   10.7581(5)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.480
_cell_measurement_theta_min      3.288
_cell_volume                     2131.94(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Single-axis Bruker MD2M diffractometer'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_wavelength     0.82654
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12144
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        29.499
_diffrn_reflns_theta_max         29.499
_diffrn_reflns_theta_min         1.643
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.0271
_exptl_absorpt_correction_T_min  0.0069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1618 before and 0.1065 after correction. The Ratio of minimum to maximum transmission is 0.2546. The \l/2 correction factor is 0.00400.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 1634 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.051(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1063P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.982
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                3416
_reflns_number_total             3506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01123d2.cif
_cod_data_source_block           bba4a
_cod_database_code               7123083
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.902
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
2.b Boron cage BH refined with riding coordinates:
 C1(H1), C2(H2), C12(H12), C13(H13), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7),
 B8(H8), B9(H9), B10(H10), B11(H11), B14(H14), B15(H15), B16(H16), B17(H17),
 B18(H18), B19(H19), B20(H20), B21(H21), B22(H22)
;
_shelx_res_checksum              93123
_olex2_submission_special_instructions 'No special instructions were received'