Synthesis of metallophophaalkenes by reaction of organometallic nucleophiles with a phosphaethynolato-borane
Wilson, Daniel; Goicoechea, Jose M.; Chemical Communications  (2019) –; doi:10.1039/C9CC03040A

data_7123454
_publ_section_title
;
 Synthesis of metallophophaalkenes by reaction of organometallic
 nucleophiles with a phosphaethynolato-borane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03040A
_journal_year                    2019
_chemical_formula_moiety         'C57 H66 Au B Fe N2 O3 P2'
_chemical_formula_sum            'C57 H66 Au B Fe N2 O3 P2'
_chemical_formula_weight         1152.68
_chemical_name_systematic
;
 (PPh3)Au(O)C[B{N(2,6-iPr-C6H3)}2(CH)2]PFe(CO)2Cp*
;
_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-2018/1
_audit_update_record
;
2019-04-18 deposited with the CCDC.    2019-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                86.392(3)
_cell_angle_beta                 73.088(4)
_cell_angle_gamma                81.048(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5793(6)
_cell_length_b                   12.6322(5)
_cell_length_c                   17.8449(6)
_cell_measurement_reflns_used    12062
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.9060
_cell_measurement_theta_min      4.3340
_cell_volume                     2679.5(2)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28840
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.214
_diffrn_reflns_theta_min         3.543
_exptl_absorpt_coefficient_mu    8.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92407
_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            orange
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         4.545
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.118
_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     617
_refine_ls_number_reflns         11081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+4.0725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9527
_reflns_number_total             11081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03040a2.cif
_cod_data_source_block           DW388_2
_cod_database_code               7123454
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.562
_shelx_estimated_absorpt_t_max   0.736
_shelx_res_checksum              41442