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_4086449
_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 H42 P2'
_chemical_formula_sum            'C32 H42 P2'
_chemical_formula_weight         488.59
_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   mixed
_audit_creation_date             2015-05-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                101.749(3)
_cell_angle_beta                 98.922(4)
_cell_angle_gamma                110.134(4)
_cell_formula_units_Z            4
_cell_length_a                   10.4449(13)
_cell_length_b                   14.5401(16)
_cell_length_c                   21.135(2)
_cell_measurement_reflns_used    7579
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.352
_cell_measurement_theta_min      2.189
_cell_volume                     2860.6(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32571
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.396
_diffrn_reflns_theta_max         25.396
_diffrn_reflns_theta_min         1.602
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0778 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.7325.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         10426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0555P)^2^+1.0494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7503
_reflns_number_total             10426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00101_si_004.cif
_cod_data_source_block           cain09_a
_cod_original_cell_volume        2860.5(6)
_cod_database_code               4086449
_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) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C45(H45A,H45B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C49(H49), C17(H17), C43(H43), C44(H44), C38(H38), C12(H12), C6(H6),
 C36(H36), C37(H37), C41(H41), C42(H42), C40(H40), C5(H5), C51(H51), C9(H9),
 C34(H34), C35(H35), C11(H11), C2(H2), C10(H10), C8(H8), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C60(H60A,H60B,H60C), C58(H58A,H58B,
 H58C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C64(H64A,H64B,H64C), C56(H56A,
 H56B,H56C), C63(H63A,H63B,H63C), C22(H22A,H22B,H22C), C62(H62A,H62B,H62C),
 C26(H26A,H26B,H26C), C59(H59A,H59B,H59C), C30(H30A,H30B,H30C), C55(H55A,H55B,
 H55C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              40840
_shelx_hkl_checksum              95142
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'