PNacPNacE: (E = Ga, In, Tl) - monomeric group 13 metal(I) heterocycles stabilized by a sterically demanding bis(iminophosphoranyl)methanide
Sindlinger, Christian P.; Lawrence, Samuel R.; Acharya, Shravan; Ohlin, C. André; Stasch, Andreas; Dalton Transactions  (2017) –; doi:10.1039/C7DT04048B

data_7044847
_publ_section_title
;
 PNacPNacE: (E = Ga, In, Tl) - monomeric group 13 metal(I) heterocycles
 stabilized by a sterically demanding bis(iminophosphoranyl)methanide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04048B
_journal_year                    2017
_chemical_formula_sum            'C49 H55 Ga I2 N2 P2'
_chemical_formula_weight         1057.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-21 deposited with the CCDC.
2017-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.37(3)
_cell_angle_beta                 88.94(3)
_cell_angle_gamma                70.95(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4770(19)
_cell_length_b                   10.759(2)
_cell_length_c                   23.466(5)
_cell_measurement_reflns_used    20883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.575
_cell_measurement_theta_min      0.868
_cell_volume                     2261.2(9)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'ADSC quantum 210r'
_diffrn_measurement_method       'f\ scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.905
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20076
_diffrn_reflns_point_group_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         28.575
_diffrn_reflns_theta_min         0.868
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       rod
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.176
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+32.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9241
_reflns_number_total             9981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04048b3.cif
_cod_data_source_block           compound4
_cod_database_code               7044847
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              81392