Synthesis and decarbonylation chemistry of gallium phosphaketenes.
Wilson, Daniel W. N.; Myers, William K.; Goicoechea, Jose M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15249–15255; doi:10.1039/d0dt03174g

data_7705675
_publ_section_title
;
 Synthesis and decarbonylation chemistry of gallium phosphaketenes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15249
_journal_page_last               15255
_journal_paper_doi               10.1039/d0dt03174g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C47 H57 Ga I N4, 0.33(C7 H8)'
_chemical_formula_sum            'C49.33 H59.67 Ga I N4'
_chemical_formula_weight         905.29
_chemical_name_systematic
;
 GaI(Me2IPr)[(NDipp)2C12H5]*0.5tol
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-08-25 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   30.5012(5)
_cell_length_b                   30.5012(5)
_cell_length_c                   25.1712(7)
_cell_measurement_reflns_used    11921
_cell_measurement_temperature    398(2)
_cell_measurement_theta_max      75.9080
_cell_measurement_theta_min      3.8490
_cell_volume                     20280.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      398(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43818
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.329
_diffrn_reflns_theta_min         3.891
_exptl_absorpt_coefficient_mu    6.484
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             8418
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 3648 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         9219
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0352P)^2^+24.0515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                8358
_reflns_number_total             9219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03174g2.cif
_cod_data_source_block           DW280
_cod_depositor_comments
'Adding full bibliography for 7705675--7705683.cif.'
_cod_original_cell_volume        20280.0(9)
_cod_database_code               7705675
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.357
_shelx_estimated_absorpt_t_max   0.738
_shelx_res_checksum              45426