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_4089685
_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         'C55 H67 N3 P Si2 Ta'
_chemical_formula_sum            'C55 H67 N3 P Si2 Ta'
_chemical_formula_weight         1038.21
_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   mixed
_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                113.594(5)
_cell_angle_beta                 97.971(5)
_cell_angle_gamma                112.323(5)
_cell_formula_units_Z            6
_cell_length_a                   19.722(5)
_cell_length_b                   21.120(5)
_cell_length_c                   22.644(5)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.27
_cell_volume                     7511(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            137218
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.095
_diffrn_reflns_theta_min         1.188
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.314
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0600 before and 0.0409 after correction. The Ratio of minimum to maximum transmission is 0.8008. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       parallelogram
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.868
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1687
_refine_ls_number_reflns         36296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+19.7416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32358
_reflns_number_total             36296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500775c_si_002.cif
_cod_data_source_block           mo_mf978_0m
_cod_depositor_comments
;

2020-06-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C165 H201 N9 P3 Si6 Ta3'
_cod_original_formula_weight         3114.64
_cod_original_formula_moiety         '3(C55 H67 N3 P Si2 Ta)'
_cod_original_formula_units_Z            2
_cod_database_code               4089685
_shelxl_version_number           2014-3
_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:
 C340(H34A,H34B,H34C), C243(H24A,H24B,H24C), C143(H14A,H14B,H14C), C313(H31A,
 H31B,H31C), C121(H12A,H12B,H12C), C352(H35A,H35B,H35C), C221(H22A,H22B,H22C),
 C152(H15A,H15B,H15C), C140(H14D,H14E,H14F), C229(H22D,H22E,H22F), C230(H23A,
 H23B,H23C), C130(H13A,H13B,H13C), C320(H32A,H32B,H32C), C321(H32D,H32E,H32F),
 C141(H14G,H14H,H14I), C138(H13D,H13E,H13F), C151(H15D,H15E,H15F), C139(H13G,
 H13H,H13I), C113(H11A,H11B,H11C), C240(H24D,H24E,H24F), C339(H33A,H33B,H33C),
 C342(H34D,H34E,H34F), C122(H12D,H12E,H12F), C131(H13J,H13K,H13L), C213(H21A,
 H21B,H21C), C251(H25A,H25B,H25C), C222(H22G,H22H,H22I), C351(H35D,H35E,H35F),
 C329(H32G,H32H,H32I), C252(H25D,H25E,H25F), C120(H12G,H12H,H12I), C238(H23D,
 H23E,H23F), C331(H33D,H33E,H33F), C231(H23G,H23H,H23I), C322(H32J,H32K,H32L),
 C338(H33G,H33H,H33I), C142(H14J,H14K,H14L), C344(H34G,H34H,H34I), C330(H33J,
 H33K,H33L), C129(H12J,H12K,H12L), C242(H24G,H24H,H24I), C220(H22J,H22K,H22L),
 C144(H14M,H14N,H14O), C239(H23J,H23K,H23L), C241(H24J,H24K,H24L), C244(H24M,
 H24N,H24O), C341(H34J,H34K,H34L), C343(H34M,H34N,H34O)
2.b Aromatic/amide H refined with riding coordinates:
 C149(H149), C111(H111), C203(H203), C216(H216), C310(H310), C247(H247),
 C127(H127), C147(H147), C348(H348), C227(H227), C333(H333), C211(H211),
 C205(H205), C210(H210), C349(H349), C208(H208), C225(H225), C327(H327),
 C102(H102), C302(H302), C136(H136), C236(H236), C347(H347), C316(H316),
 C110(H110), C105(H105), C106(H106), C148(H148), C104(H104), C334(H334),
 C249(H249), C204(H204), C118(H118), C311(H311), C108(H108), C305(H305),
 C206(H206), C248(H248), C234(H234), C304(H304), C137(H137), C233(H233),
 C202(H202), C325(H325), C318(H318), C125(H125), C134(H134), C306(H306),
 C308(H308), C218(H218), C116(H116), C303(H303), C103(H103), C336(H336)
;
_olex2_submission_special_instructions 'No special instructions were received'