Synthesis of a Tris(phosphaalkene)phosphine Ligand and Fundamental Organometallic Reactions on Its Sterically Shielded Metal Complexes
Miura-Akagi, Preston M.; Nakashige, Mika L.; Maile, Caitlin K.; Oshiro, Shelly M.; Gurr, Joshua R.; Yoshida, Wesley Y.; Royappa, A. Timothy; Krause, Colleen E.; Rheingold, Arnold L.; Hughes, Russell P.; Cain, Matthew F.; Organometallics 35 (2016) 2224–; doi:10.1021/acs.organomet.6b00250

data_4086583
_publ_contact_author_name
;
;
_publ_section_title
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 Synthesis of a Tris(phosphaalkene)phosphine Ligand and Fundamental
 Organometallic Reactions on Its Sterically Shielded Metal Complexes
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_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2224
_journal_paper_doi               10.1021/acs.organomet.6b00250
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C75 H102 P4'
_chemical_formula_sum            'C75 H102 P4'
_chemical_formula_weight         1127.44
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.536(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5848(5)
_cell_length_b                   24.3520(8)
_cell_length_c                   23.4755(8)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.46
_cell_measurement_theta_min      3.87
_cell_volume                     7751.3(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            58604
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         68.727
_diffrn_reflns_theta_min         2.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0572 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.4150.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         14080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+4.4608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12194
_reflns_number_total             14080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00250_si_002.cif
_cod_data_source_block           cain01_sq
_cod_database_code               4086583
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.731
_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. Others
 Sof(C44')=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45')=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=Sof(C46')=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
3.a Me refined with riding coordinates:
 C44(H44A,H44B,H44C), C44'(H44D,H44E,H44F), C45(H45A,H45B,H45C), C45'(H45D,
 H45E,H45F), C46(H46A,H46B,H46C), C46'(H46D,H46E,H46F)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C26(H26),
 C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C37(H37), C51(H51), C54(H54),
  C55(H55), C56(H56), C57(H57), C60(H60), C62(H62)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C)
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_shelx_res_checksum              29886
_shelx_hkl_checksum              84385
_shelx_fab_checksum              74255
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'