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_4344695
_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 H69 N6 O12 P S, 3(C7 H8), C2 H6 O'
_chemical_formula_sum            'C83 H99 N6 O13 P S'
_chemical_formula_weight         1451.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 115.95(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.233(12)
_cell_length_b                   18.704(7)
_cell_length_c                   25.634(9)
_cell_measurement_reflns_used    92468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.553
_cell_measurement_theta_min      2.681
_cell_volume                     16483(11)
_computing_cell_refinement       MARHKL
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_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
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;

'MERCURY (Macrae et al., 2008), Platon (Spek, 2009)'
;
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '120 images, \D\F 2.0\% '
_diffrn_radiation_monochromator  Zr-filter
_diffrn_radiation_source         'RU200  rotating anode'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            92468
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        23.553
_diffrn_reflns_theta_max         23.553
_diffrn_reflns_theta_min         2.681
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       plate
_exptl_crystal_F_000             6192
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0022(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     927
_refine_ls_number_reflns         12162
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1633P)^2^+33.3127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2353
_refine_ls_wR_factor_ref         0.2481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10075
_reflns_number_total             12162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02750_si_002.cif
_cod_data_source_block           ig252_kr
_cod_database_code               4344695
_shelxl_version_number           2014-3
_shelx_res_checksum              65265
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