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_7123455
_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         'C42 H60 B Fe N2 O3 P Si, 0.25(C6 H14)'
_chemical_formula_sum            'C43.5 H63.5 B Fe N2 O3 P Si'
_chemical_formula_weight         788.18
_chemical_name_systematic
;
 (Me3Si)OC[B{N(2,6-iPr-C6H3)}2(CH)2]PFe(CO)2Cp*_0.25hex
;
_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                78.827(4)
_cell_angle_beta                 86.973(4)
_cell_angle_gamma                78.977(4)
_cell_formula_units_Z            4
_cell_length_a                   12.6726(7)
_cell_length_b                   14.4208(6)
_cell_length_c                   25.6379(10)
_cell_measurement_reflns_used    10974
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.4140
_cell_measurement_theta_min      3.5070
_cell_volume                     4511.1(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.973
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            39615
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.356
_diffrn_reflns_theta_min         3.178
_exptl_absorpt_coefficient_mu    3.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93373
_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    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             1690
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     963
_refine_ls_number_reflns         18631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0725P)^2^+1.7557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14547
_reflns_number_total             18631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03040a2.cif
_cod_data_source_block           DW288B
_cod_original_formula_sum        'C43.50 H63.50 B Fe N2 O3 P Si'
_cod_database_code               7123455
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.718
_shelx_estimated_absorpt_t_max   0.764
_shelx_res_checksum              97992