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_7705680
_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         'C57 H64 Ga I N4, 2(C7 H8)'
_chemical_formula_sum            'C71 H80 Ga I N4'
_chemical_formula_weight         1186.01
_chemical_name_systematic
;
 GaI(IMes)[(NDipp)2C12H5]*2tol
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   13.65400(10)
_cell_length_b                   18.29020(10)
_cell_length_c                   24.71570(10)
_cell_measurement_reflns_used    40115
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.9900
_cell_measurement_theta_min      4.0120
_cell_volume                     6172.36(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.243
_diffrn_reflns_theta_min         3.698
_exptl_absorpt_coefficient_mu    4.861
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       rod
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 5358 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0270(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         12864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.9451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                12373
_reflns_number_total             12864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03174g2.cif
_cod_data_source_block           DW311_B
_cod_depositor_comments
'Adding full bibliography for 7705675--7705683.cif.'
_cod_database_code               7705680
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.697
_shelx_estimated_absorpt_t_max   0.829
_shelx_res_checksum              20318