Synthesis and Characterization of the Monomeric Imides Ar'MNAr'' (M = Ga or In; Ar' or Ar'' = Terphenyl Ligands) with Two-Coordinate Gallium and Indium
Robert J. Wright; Andrew D. Phillips; Thomas L. Allen; William H. Fink; Philip P. Power; Journal of the American Chemical Society 125 (2003) 1694–1695; doi:10.1021/ja029422u

data_4113466
_publ_section_title
;
 Synthesis and Characterization of the Monomeric Imides Ar'MNAr'' (M = Ga
 or In; Ar' or Ar'' = Terphenyl Ligands) with Two-Coordinate Gallium and
 Indium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1694
_journal_page_last               1695
_journal_paper_doi               10.1021/ja029422u
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C60 H74 N6'
_chemical_formula_weight         879.25
_chemical_name_common            tBuJeff*N3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.868(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.9918(19)
_cell_length_b                   6.3325(5)
_cell_length_c                   32.709(2)
_cell_measurement_reflns_used    912
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      61.531
_cell_measurement_theta_min      5.698
_cell_volume                     5149.4(6)
_computing_cell_refinement       'Bruker SAINT 6.35A (2002)'
_computing_data_collection       'Bruker SMART 5.054 (2001)'
_computing_data_reduction        'Bruker SAINT 6.35A (2002)'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            46430
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time
; 
frames measured at beginning and end of data collection 
;
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.9772
_exptl_absorpt_correction_T_min  0.9625
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1335P)^2^+3.0154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2196
_reflns_number_gt                6897
_reflns_number_total             9338
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ja029422u_s1.cif
_cod_data_source_block           adp35
_cod_original_cell_volume        5149.4(7)
_cod_database_code               4113466