7-Metalla-1,4-diphosphanorbornadienes: cycloaddition of monovalent group 13 NacNac complexes to a stable 1,4-diphosphinine.
Koner, Abhishek; Gabidullin, Bulat M.; Kelemen, Zsolt; Nyulászi, László; Nikonov, Georgii I.; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8248–8253; doi:10.1039/c9dt01425j

data_7700011
_publ_section_title
;
 7-Metalla-1,4-diphosphanorbornadienes: cycloaddition of monovalent group
 13 NacNac complexes to a stable 1,4-diphosphinine.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8248
_journal_page_last               8253
_journal_paper_doi               10.1039/c9dt01425j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C51 H77 Ga N6 P2 S2'
_chemical_formula_weight         969.96
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-02-28 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.684(3)
_cell_length_b                   12.5765(17)
_cell_length_c                   17.783(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      2.63
_cell_volume                     5296.9(13)
_computing_cell_refinement       'APEX II (Bruker, 2009)'
_computing_data_collection       'APEX II (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54651
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.276
_diffrn_reflns_theta_min         1.720
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ether'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 4645 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         16035
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.1665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.896
_reflns_number_gt                12026
_reflns_number_total             16035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01425j2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7700010--7700011.cif.'
_cod_database_code               7700011
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.792
_shelx_estimated_absorpt_t_max   0.867
_shelx_res_checksum              10547