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_1560005
_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 H47 Au Cl2 N3 P3 Ti, 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C29 H49 Au Cl4 N3 P3 Ti'
_chemical_formula_weight         919.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-27
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2921(8)
_cell_length_b                   13.7871(7)
_cell_length_c                   18.9179(10)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.564
_cell_measurement_theta_min      2.955
_cell_volume                     3727.7(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer triump Mo'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_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  0.0268
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65977
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         2.850
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_exptl_absorpt_coefficient_mu    4.585
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.2024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0600 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.7737.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of dichloromethane and pentane  by slow evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0055P)^2^+11.9888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4161
_reflns_number_total             4478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04736h2.cif
_cod_data_source_block           7b
_cod_depositor_comments
'Adding full bibliography for 1560000--1560012.cif.'
_cod_database_code               1560005
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.632
_shelx_estimated_absorpt_t_min   0.261
_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. Restrained distances
 C2-C3 = C3-C4 = C4-C2
 2.44353 with sigma of 0.02
 C1-C2 = C1-C3 = C1-C4
 1.4936 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C1(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) H17A(0.5) H17B(0.5)
 Fixed U12: C1(0)
 Fixed U23: C1(0)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              27311
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'