Reappraising Schmidpeter's bis(iminophosphoranyl)phosphides: coordination to transition metals and bonding analysis.
Normand, Adrien T.; Sosa Carrizo, E. Daiann; Magnoux, Corentin; Lobato, Esteban; Cattey, Hélène; Richard, Philippe; Brandès, Stéphane; Devillers, Charles H.; Romieu, Anthony; Le Gendre, Pierre; Fleurat-Lessard, Paul; Chemical science 12 (2020) 253–269; doi:10.1039/d0sc04736h

data_1560000
_publ_section_title
;
 Reappraising Schmidpeter's bis(iminophosphoranyl)phosphides: coordination
 to transition metals and bonding analysis.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              253
_journal_page_last               269
_journal_paper_doi               10.1039/d0sc04736h
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C28 H46 Li N2 O P3'
_chemical_formula_sum            'C28 H46 Li N2 O P3'
_chemical_formula_weight         526.52
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-19 deposited with the CCDC.	2020-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.107(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.215(4)
_cell_length_b                   30.038(9)
_cell_length_c                   10.723(4)
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.94
_cell_volume                     2954.5(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 Venture triumph Mo'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            48835
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.6468
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0516 before and 0.0418 after correction. The Ratio of minimum to maximum transmission is 0.9482. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_recrystallization_method
'The material was recrystallised from pentane by slow evaporation'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.025
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0873P)^2^+7.4284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5996
_reflns_number_total             6783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04736h2.cif
_cod_data_source_block           2b'
_cod_depositor_comments
'Adding full bibliography for 1560000--1560012.cif.'
_cod_original_cell_volume        2954.5(18)
_cod_database_code               1560000
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.928
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(C1D) = Uiso(C1E) = Uiso(C1A) = Uiso(C1H)
Uiso(C1G) = Uiso(C1B) = Uiso(C1F) = Uiso(C1C)
Uiso(O1) = Uiso(O2)
3. Others
 Fixed Sof: H7A(0.62) H7B(0.38) C8(0.63) H8A(0.63) H8B(0.63) H8C(0.63)
 C8A(0.37) H8AA(0.37) H8AB(0.37) H8AC(0.37) C10(0.63) H10(0.63) C10A(0.37)
 H10A(0.37) C11(0.63) H11A(0.63) H11B(0.63) H11C(0.63) C11A(0.37) H11D(0.37)
 H11E(0.37) H11F(0.37) H12A(0.62) H12B(0.62) H12C(0.62) H12D(0.38) H12E(0.38)
 H12F(0.38) O2(0.63) C1A(0.63) H1AA(0.63) H1AB(0.63) C1B(0.63) H1BA(0.63)
 H1BB(0.63) C1C(0.63) H1CA(0.63) H1CB(0.63) C1D(0.63) H1DA(0.63) H1DB(0.63)
 O1(0.37) C1E(0.37) H1EA(0.37) H1EB(0.37) C1F(0.37) H1FA(0.37) H1FB(0.37)
 C1G(0.37) H1GA(0.37) H1GB(0.37) C1H(0.37) H1HA(0.37) H1HB(0.37)
4.a Free rotating group:
 O2(C1A,C1B,C1C,C1D), O1(C1E,C1F,C1G,C1H)
4.b Ternary CH refined with riding coordinates:
 C7(H7A), C7(H7B), C10(H10), C10A(H10A), C13(H13), C16(H16)
4.c Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,
 H1EB), C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1H(H1HA,H1HB)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C11A(H11D,H11E,H11F), C12(H12A,H12B,H12C), C12(H12D,H12E,H12F), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              58129
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'