1,1′-Bifunctional Aminophosphane Complexes via N‒H Bond Insertions of a Li/Cl Phosphinidenoid Complex and First Studies on N/P Mono Functionalizations
Streubel, Rainer; Schmer, Alexander; Kyri, Andreas W.; Schnakenburg, Gregor; Organometallics  (2017) –; doi:10.1021/acs.organomet.7b00073

data_4087217
_publ_section_title
;
 1,1&#x2032;-Bifunctional Aminophosphane Complexes via N--H Bond
 Insertions of a Li/Cl Phosphinidenoid Complex and First Studies on N/P
 Mono Functionalizations
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.7b00073
_journal_year                    2017
_chemical_formula_moiety         'C28 H26 N O5 P W'
_chemical_formula_sum            'C28 H26 N O5 P W'
_chemical_formula_weight         671.32
_chemical_name_systematic
;
 ?
;
_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             2017-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                104.204(3)
_cell_angle_beta                 98.484(3)
_cell_angle_gamma                104.184(3)
_cell_formula_units_Z            4
_cell_length_a                   10.7367(7)
_cell_length_b                   15.6770(10)
_cell_length_c                   17.4538(10)
_cell_measurement_reflns_used    3857
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.08
_cell_measurement_theta_min      2.80
_cell_volume                     2692.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13114
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.234
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.386
_exptl_absorpt_correction_T_max  0.263805
_exptl_absorpt_correction_T_min  0.07344
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1479 before and 0.0514 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1616 before and 0.0848 after correction.
 The Ratio of minimum to maximum transmission is 0.28.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 50360 reflections, Rint = 0.0700
 (30863 with I > 3sig(I), Rint = 0.0658)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.503
_refine_diff_density_min         -2.349
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         13114
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+25.2131P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10885
_reflns_number_total             13114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00073_si_002.cif
_cod_data_source_block           2986
_cod_database_code               4087217
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.309
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8045(12) 0.1955(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2: within 2A with sigma of 0.007 and sigma for terminal
atoms of 0.014
N2 \\sim C31 \\sim C32 \\sim C29 \\sim C30: within 2A with sigma of 0.007 and
sigma for terminal atoms of 0.014
Uanis(C25) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C29(H29A,H29B), C31(H31A,H31B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              41274
_shelx_hkl_checksum              54011
_olex2_submission_special_instructions 'No special instructions were received'