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_4089683
_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         'C52 H56 N2 P Ta'
_chemical_formula_sum            'C52 H56 N2 P Ta'
_chemical_formula_weight         920.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1759(4)
_cell_length_b                   33.5707(11)
_cell_length_c                   12.7008(4)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.043
_cell_measurement_theta_min      2.563
_cell_volume                     4705.1(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33385
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.404
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0522 before and 0.0411 after correction. The Ratio of minimum to maximum transmission is 0.8820. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+1.3533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                6617
_reflns_number_total             8328
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500775c_si_002.cif
_cod_data_source_block           mf904_0m
_cod_database_code               4089683
_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,H,H,H) groups
2. Others
 Fixed Sof: H13A(0.5) H13B(0.5) H13C(0.5) H13D(0.5) H13E(0.5) H13F(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) H20D(0.5) H20E(0.5) H20F(0.5) H21A(0.5)
 H21B(0.5) H21C(0.5) H21D(0.5) H21E(0.5) H21F(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) H22D(0.5) H22E(0.5) H22F(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
 H29D(0.5) H29E(0.5) H29F(0.5) H30A(0.5) H30B(0.5) H30C(0.5) H30D(0.5)
 H30E(0.5) H30F(0.5) H31A(0.5) H31B(0.5) H31C(0.5) H31D(0.5) H31E(0.5)
 H31F(0.5) H38A(0.5) H38B(0.5) H38C(0.5) H38D(0.5) H38E(0.5) H38F(0.5)
 H39A(0.5) H39B(0.5) H39C(0.5) H39D(0.5) H39E(0.5) H39F(0.5) H44A(0.5)
 H44B(0.5) H44C(0.5) H44D(0.5) H44E(0.5) H44F(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C43(H43A,H43B)
3.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),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
3.c Disordered Me refined with riding coordinates:
 C13(H13A,H13B,H13C,H13D,H13E,H13F), C20(H20A,H20B,H20C,H20D,H20E,H20F),
 C21(H21A,H21B,H21C,H21D,H21E,H21F), C22(H22A,H22B,H22C,H22D,H22E,H22F),
 C29(H29A,H29B,H29C,H29D,H29E,H29F), C30(H30A,H30B,H30C,H30D,H30E,H30F),
 C31(H31A,H31B,H31C,H31D,H31E,H31F), C38(H38A,H38B,H38C,H38D,H38E,H38F),
 C39(H39A,H39B,H39C,H39D,H39E,H39F), C44(H44A,H44B,H44C,H44D,H44E,H44F)
;
_olex2_submission_special_instructions 'No special instructions were received'