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_4089681
_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 H49 Cl N2 P Ta, C6 H6'
_chemical_formula_sum            'C50 H55 Cl N2 P Ta'
_chemical_formula_weight         931.34
_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             2014-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                85.154(2)
_cell_angle_beta                 75.726(2)
_cell_angle_gamma                62.928(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2733(5)
_cell_length_b                   13.1929(5)
_cell_length_c                   18.2941(8)
_cell_measurement_reflns_used    8084
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.232
_cell_measurement_theta_min      2.433
_cell_volume                     2554.89(19)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32636
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0553 before and 0.0410 after correction. The Ratio of minimum to maximum transmission is 0.8045. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1.7587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                8555
_reflns_number_total             9163
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500775c_si_002.cif
_cod_data_source_block           mf822_0m
_cod_depositor_comments
;

2020-09-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         465.67
_cod_original_formula_moiety         '0.5(C44 H49 Cl N2 P Ta), 0.5(C6 H6)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        2554.89(18)
_cod_original_formula_sum        'C25 H27.50 Cl0.50 N P0.50 Ta0.50'
_cod_database_code               4089681
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H02(0.027) H03(0.036) H04(0.039) H05(0.04) H06(0.029) H08(0.022)
 H10(0.026) H11(0.024) H13A(0.038) H13B(0.038) H13C(0.038) H16(0.026)
 H18(0.029) H20A(0.035) H20B(0.035) H20C(0.035) H21A(0.037) H21B(0.037)
 H21C(0.037) H22A(0.057) H22B(0.057) H22C(0.057) H25(0.032) H27(0.033)
 H29A(0.04) H29B(0.04) H29C(0.04) H30A(0.038) H30B(0.038) H30C(0.038)
 H31A(0.067) H31B(0.067) H31C(0.067) H33(0.023) H34(0.023) H36(0.023)
 H38A(0.042) H38B(0.042) H38C(0.042) H39A(0.051) H39B(0.051) H39C(0.051)
 H40A(0.032) H40B(0.032) H43A(0.027) H43B(0.027) H44A(0.046) H44B(0.046)
 H44C(0.046) H907(0.044) H908(0.041) H909(0.042) H910(0.038) H911(0.041)
 H912(0.047)
 Fixed X: H02(0.8452) H03(1.0366) H04(1.2224) H05(1.2179) H06(1.0271)
 H08(0.8452) H10(0.8038) H11(0.737) H13A(0.8958) H13B(0.9536) H13C(0.8117)
 H16(0.5575) H18(0.9066) H20A(0.9237) H20B(0.9619) H20C(1.0126) H21A(0.5024)
 H21B(0.4846) H21C(0.4228) H22A(0.6569) H22B(0.8062) H22C(0.7479) H25(0.1781)
 H27(0.478) H29A(0.7011) H29B(0.6625) H29C(0.6994) H30A(0.3458) H30B(0.2381)
 H30C(0.2193) H31A(0.144) H31B(0.2599) H31C(0.2332) H33(0.4053) H34(0.4198)
 H36(0.7266) H38A(0.5114) H38B(0.6611) H38C(0.574) H39A(0.704) H39B(0.662)
 H39C(0.8071) H40A(0.7599) H40B(0.6146) H43A(0.9934) H43B(0.926) H44A(1.0678)
 H44B(0.9274) H44C(0.9946) H907(0.7183) H908(0.5775) H909(0.517) H910(0.5953)
 H911(0.7328) H912(0.7955)
 Fixed Y: H02(0.4492) H03(0.4562) H04(0.3046) H05(0.1443) H06(0.135)
 H08(0.2496) H10(-0.0298) H11(-0.0381) H13A(0.179) H13B(0.0433) H13C(0.1216)
 H16(-0.1509) H18(-0.2356) H20A(0.0134) H20B(-0.061) H20C(-0.1209) H21A(0.1194)
 H21B(0.0125) H21C(0.072) H22A(-0.3198) H22B(-0.3829) H22C(-0.318) H25(0.5854)
 H27(0.5803) H29A(0.4387) H29B(0.5532) H29C(0.4352) H30A(0.4371) H30B(0.4338)
 H30C(0.5514) H31A(0.6717) H31B(0.6138) H31C(0.731) H33(0.6291) H34(0.7325)
 H36(0.4588) H38A(0.7543) H38B(0.6807) H38C(0.6415) H39A(-0.0088) H39B(0.0119)
 H39C(-0.0338) H40A(0.1422) H40B(0.188) H43A(0.1478) H43B(0.2752) H44A(0.1529)
 H44B(0.2037) H44C(0.0763) H907(0.1917) H908(0.1774) H909(0.0323) H910(-0.0978)
 H911(-0.0822) H912(0.0617)
 Fixed Z: H02(0.768) H03(0.7232) H04(0.7416) H05(0.8033) H06(0.8474)
 H08(0.9873) H10(1.061) H11(0.9545) H13A(1.1028) H13B(1.1066) H13C(1.1507)
 H16(0.846) H18(0.7179) H20A(0.764) H20B(0.6889) H20C(0.7615) H21A(0.9112)
 H21B(0.9493) H21C(0.88) H22A(0.7743) H22B(0.7646) H22C(0.6952) H25(0.7184)
 H27(0.5639) H29A(0.6769) H29B(0.6304) H29C(0.59) H30A(0.8591) H30B(0.8262)
 H30C(0.8582) H31A(0.6032) H31B(0.5322) H31C(0.5692) H33(0.8239) H34(0.9141)
 H36(0.9538) H38A(1.0065) H38B(0.9881) H38C(1.0519) H39A(0.5539) H39B(0.6435)
 H39C(0.6009) H40A(0.5401) H40B(0.5827) H43A(0.6707) H43B(0.6432) H44A(0.5392)
 H44B(0.5279) H44C(0.5555) H907(0.3027) H908(0.243) H909(0.2738) H910(0.3648)
 H911(0.4254) H912(0.394)
;
_olex2_submission_special_instructions 'No special instructions were received'