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_4089684
_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         'C44 H50 N2 P Ta'
_chemical_formula_sum            'C44 H50 N2 P Ta'
_chemical_formula_weight         818.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                79.960(5)
_cell_angle_beta                 87.070(5)
_cell_angle_gamma                84.776(5)
_cell_formula_units_Z            2
_cell_length_a                   9.038(5)
_cell_length_b                   11.789(5)
_cell_length_c                   17.915(5)
_cell_measurement_reflns_used    8150
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.008
_cell_measurement_theta_min      2.264
_cell_volume                     1870.6(14)
_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-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23892
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.014
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0631 before and 0.0362 after correction. The Ratio of minimum to maximum transmission is 0.7363. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+1.5397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                6177
_reflns_number_total             6567
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500775c_si_002.cif
_cod_data_source_block           mo_mf919_0m
_cod_database_code               4089684
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C34(H34), C25(H25), C10(H10), C03(H03), C33(H33), C27(H27),
 C08(H08), C06(H06), C11(H11), C02(H02), C04(H04), C05(H05), C16(H16), C18(H18)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C13(H13A,H13B,
 H13C), C38(H38A,H38B,H38C), C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C44(H44A,
 H44B,H44C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C)
;
_olex2_submission_special_instructions 'No special instructions were received'