Synthesis and Structural Studies of Gallium(III) and Iron(III) Hemicryptophane Complexes.
Gosse, Isabelle; Robeyns, Koen; Bougault, Catherine; Martinez, Alexandre; Tinant, Bernard; Dutasta, Jean-Pierre; Inorganic chemistry 55 (2016) 1011–1013; doi:10.1021/acs.inorgchem.5b02750

data_4344696
_publ_section_title
;
 Synthesis and Structural Studies of Gallium(III) and Iron(III)
 Hemicryptophane Complexes.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1011
_journal_page_last               1013
_journal_paper_doi               10.1021/acs.inorgchem.5b02750
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C60 H66 Fe N6 O12 P S'
_chemical_formula_sum            'C60 H66 Fe N6 O12 P S'
_chemical_formula_weight         1182.06
_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
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                79.22(2)
_cell_angle_beta                 81.96(2)
_cell_angle_gamma                61.53(2)
_cell_formula_units_Z            2
_cell_length_a                   12.050(5)
_cell_length_b                   12.144(5)
_cell_length_c                   23.020(9)
_cell_measurement_reflns_used    30382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.481
_cell_measurement_theta_min      2.561
_cell_volume                     2904(2)
_computing_cell_refinement       MARHKL
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_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material
;

'MERCURY (Macrae et al., 2008), Platon (Spek, 2009)'
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.743
_diffrn_measured_fraction_theta_max 0.743
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '76 images, \D\F 3.0\% '
_diffrn_radiation_monochromator  Zr-filter
_diffrn_radiation_source         'RU200  rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.743
_diffrn_reflns_Laue_measured_fraction_max 0.743
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_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30382
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.743
_diffrn_reflns_theta_full        22.480
_diffrn_reflns_theta_max         22.481
_diffrn_reflns_theta_min         2.561
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         5619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0707
_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^)+(0.1186P)^2^+6.6065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.2059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4589
_reflns_number_total             5619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02750_si_002.cif
_cod_data_source_block           fer
_cod_database_code               4344696
_shelxl_version_number           2014-3
_shelx_res_checksum              24080
_shelx_hkl_checksum              83650
_shelx_fab_checksum              71682