Carbon‒Carbon Bond Forming Reactions with Tantalum Diamidophosphine Complexes That Incorporate Alkyne Ligands
Parker, Kyle D. J.; Fryzuk, Michael D.; Organometallics 33 (2014) 6122–; doi:10.1021/om500775c

data_4089682
_publ_section_title
;
 Carbon--Carbon Bond Forming Reactions with Tantalum Diamidophosphine
 Complexes That Incorporate Alkyne Ligands
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6122
_journal_paper_doi               10.1021/om500775c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C46 H57 Cl N2 P Si2 Ta'
_chemical_formula_sum            'C46 H57 Cl N2 P Si2 Ta'
_chemical_formula_weight         941.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 108.045(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   12.175(5)
_cell_length_b                   20.580(5)
_cell_length_c                   18.273(5)
_cell_measurement_reflns_used    7860
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.40
_cell_volume                     4353(2)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.609
_diffrn_reflns_theta_min         1.534
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.712
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1069 before and 0.0697 after correction. The Ratio of minimum to maximum transmission is 0.7378. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         10050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+9.0088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9189
_reflns_number_total             10050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500775c_si_002.cif
_cod_data_source_block           mf878_0m
_cod_database_code               4089682
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C38(H38A,
 H38B,H38C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
2.b Aromatic/amide H refined with riding coordinates:
 C02(H02), C03(H03), C04(H04), C05(H05), C06(H06), C08(H08), C10(H10),
 C11(H11), C16(H16), C18(H18), C25(H25), C27(H27), C33(H33), C34(H34), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'