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_7020116
_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(Ga C12 O6 H24), 4(Al F36 O4 C16), 9(C6 H5 F)'
_chemical_formula_sum            'C166 H141 Al4 F153 Ga4 O40'
_chemical_formula_weight         6069.88
_chemical_name_common            (Ga(18-crown-6)(PhF)2)2(Al(OC(CF3)3)4)2.0.5PhF
_chemical_name_systematic
'[Ga(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             2012-01-18
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0003(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.7737(7)
_cell_length_b                   15.8400(6)
_cell_length_c                   35.5352(12)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.0251
_cell_measurement_theta_min      2.4380
_cell_volume                     11069.2(7)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
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.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            99060
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_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    0.695
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6513
_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    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.148
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1980
_refine_ls_number_reflns         22436
_refine_ls_number_restraints     7127
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+39.0146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2049
_reflns_number_gt                16948
_reflns_number_total             22436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30379e.txt
_cod_data_source_block           input2
_cod_database_code               7020116