Streamlined Preparation and Coordination Chemistry of Hybrid Phosphine–Phosphaalkene Ligands
Magnuson, Kevin W.; Oshiro, Shelly M.; Gurr, Joshua R.; Yoshida, Wesley Y.; Gembicky, Milan; Rheingold, Arnold L.; Hughes, Russell P.; Cain, Matthew F.; Organometallics 35 (2016) 855–859; doi:10.1021/acs.organomet.6b00101

data_4086451
_publ_contact_author_name
;
;
_publ_section_title
;
 Streamlined Preparation and Coordination Chemistry of Hybrid
 Phosphine--Phosphaalkene Ligands
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              855
_journal_page_last               859
_journal_paper_doi               10.1021/acs.organomet.6b00101
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C32 H54 P2'
_chemical_formula_sum            'C32 H54 P2'
_chemical_formula_weight         500.69
_chemical_name_common            SO7
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                101.584(4)
_cell_angle_beta                 109.156(4)
_cell_angle_gamma                99.100(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8594(12)
_cell_length_b                   11.7510(16)
_cell_length_c                   14.647(2)
_cell_measurement_reflns_used    4945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.20
_cell_volume                     1523.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7168
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         1.529
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0619 before and 0.0436 after correction.
The Ratio of minimum to maximum transmission is 0.6518.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         7168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0469P)^2^+0.5630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6211
_reflns_number_total             7168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00101_si_006.cif
_cod_data_source_block           cain02
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 4609 2016-04-01 06:22:49Z antanas 
;
_cod_database_code               4086451
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7815(9) 0.2185(9)
2. 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
3. Others
 Sof(C26')=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27')=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
4.c Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C26'(H26D,H26E,H26F), C27(H27A,H27B,H27C), C27'(H27D,H27E,H27F),
 C28(H28A,H28B,H28C), C28'(H28D,H28E,H28F), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C17(H17), C19(H19)
;
_shelx_res_checksum              23406
_shelx_hkl_checksum              22795
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'