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_1560001
_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
'C56 H94 Br2 Cl2 Cu2 N6 P6 Ti2, 2.28(C H2 Cl2)'
_chemical_formula_sum            'C58.28 H98.56 Br2 Cl6.56 Cu2 N6 P6 Ti2'
_chemical_formula_weight         1684.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-14
_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                 90.810(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6149(6)
_cell_length_b                   16.6838(8)
_cell_length_c                   20.0416(9)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.97
_cell_volume                     3883.3(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 0.998
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51118
_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         27.585
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-90C'
_exptl_absorpt_coefficient_mu    2.155
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0779 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.8248.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and pentane  by slow evaporation'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.193
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0341P)^2^+14.0897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6922
_reflns_number_total             8943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04736h2.cif
_cod_data_source_block           8b
_cod_depositor_comments
'Adding full bibliography for 1560000--1560012.cif.'
_cod_database_code               1560001
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.511
_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. Others
 Fixed Sof: C13(0.52) C13A(0.48) C14(0.52) H14(0.52) C14A(0.48) H14A(0.48)
 C15(0.52) H15(0.52) C15A(0.48) H15A(0.48) C16(0.52) H16(0.52) C16A(0.48)
 H16A(0.48) C17(0.52) H17(0.52) C17A(0.48) H17A(0.48) C18(0.52) H18(0.52)
 C18A(0.48) H18A(0.48) Cl2A(0.5) Cl3A(0.5) C29A(0.5) H29A(0.5) H29B(0.5)
 Cl2(0.5) Cl3(0.5) C29(0.5) H29C(0.5) H29D(0.5) Cl4(0.14) Cl5(0.14) C30(0.14)
 H30A(0.14) H30B(0.14)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
3.b Secondary CH2 refined with riding coordinates:
 C29A(H29A,H29B), C29(H29C,H29D), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C14(H14), C14A(H14A), C15A(H15A),
 C16(H16), C16A(H16A), C17(H17), C17A(H17A), C18(H18), C18A(H18A)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              7026
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'