Synthesis and Structural Characterization of Some Monomeric Group 13 Amides
Joel S. Silverman; Claire J. Carmalt; Alan H. Cowley; Robert D. Culp; Richard A. Jones; Brian G. McBurnett; Inorganic Chemistry 38 (1999) 296–300; doi:10.1021/ic980619q

data_4321740
_publ_section_title
;
 Synthesis and Structural Characterization of Some Monomeric Group 13
 Amides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              296
_journal_page_last               300
_journal_paper_doi               10.1021/ic980619q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C54 H90 In N3'
_chemical_formula_weight         896.11
_chemical_name_systematic
; 
     Tris[(2,4,6-tri-t-butylphenyl)amido]indium(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.564(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.463(2)
_cell_length_b                   11.9740(10)
_cell_length_c                   31.179(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.29
_cell_measurement_theta_min      4.79
_cell_volume                     5290.0(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            11315
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        5.63
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.8575
_exptl_absorpt_correction_T_min  0.5891
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.813
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0037(4)
_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_all   1.583
_refine_ls_goodness_of_fit_obs   1.842
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.603
_refine_ls_restrained_S_obs      1.842
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_obs          0.0790
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2167
_refine_ls_wR_factor_obs         0.1944
_reflns_number_observed          5757
_reflns_number_total             9170
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980619q_1.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321740