Isolated cationic crown ether complexes of gallium(I) and indium(I).
Higelin, Alexander; Haber, Christoph; Meier, Stefan; Krossing, Ingo; Dalton transactions (Cambridge, England : 2003) 41 (2012) 12011–12015; doi:10.1039/c2dt30379e

data_7020115
_publ_section_title
;
 Isolated cationic crown ether complexes of gallium(I) and indium(I).
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12011
_journal_page_last               12015
_journal_paper_doi               10.1039/c2dt30379e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'4(In C12 O6 H24), 4(Al F36 O4 C16), 9(C6 H5 F)'
_chemical_formula_sum            'C166 H141 Al4 F153 In4 O40'
_chemical_formula_weight         6249.82
_chemical_name_common            (In(18-crown-6)(PhF)2)2(Al(OC(CF3)3)4)2.0.5PhF
_chemical_name_systematic
'[In(18-crown-6)(PhF)2]2[Al(OC(CF3)3)4]2.0.5PhF'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-01-05
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.9320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.7449(3)
_cell_length_b                   15.9218(2)
_cell_length_c                   35.6744(6)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.945
_cell_measurement_theta_min      2.304
_cell_volume                     11155.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'double mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            75318
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'ImuS microsource'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0862 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.8687.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5648
_exptl_crystal_preparation       perfluoroetheroil
_exptl_crystal_recrystallization_method fluorobenzene
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2111
_refine_ls_number_reflns         24937
_refine_ls_number_restraints     3408
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+31.1683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                19041
_reflns_number_total             24937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30379e.txt
_cod_data_source_block           input
_cod_database_code               7020115