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_1560006
_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         '4(C36 H30 Cl3 N2 P3 Zr), 3(C H2 Cl2)'
_chemical_formula_sum            'C147 H126 Cl18 N8 P12 Zr4'
_chemical_formula_weight         3379.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-11
_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                82.319(4)
_cell_angle_beta                 80.357(5)
_cell_angle_gamma                70.217(4)
_cell_formula_units_Z            1
_cell_length_a                   11.8938(12)
_cell_length_b                   12.0699(11)
_cell_length_c                   27.548(3)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.522
_cell_measurement_theta_min      2.961
_cell_volume                     3656.1(6)
_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
_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 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  0.0270
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.997
_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       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            106171
_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         27.539
_diffrn_reflns_theta_min         2.958
_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    0.791
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0525 before and 0.0415 after correction.
The Ratio of minimum to maximum transmission is 0.9233.
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    1.535
_exptl_crystal_description       prism
_exptl_crystal_F_000             1710
_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          0.32
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         16785
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0265P)^2^+4.1469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14964
_reflns_number_total             16785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04736h2.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 1560000--1560012.cif.'
_cod_database_code               1560006
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl9-Cl10
 2.916 with sigma of 0.03
 Cl9-C74 = Cl10-C74
 1.771 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl9 \\sim Cl10 \\sim C74: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl9, Cl10, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl9(0.5) Cl10(0.5) C74(0.5) H74A(0.5) H74B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C38(H38), C46(H46), C18(H18), C68(H68), C20(H20), C6(H6),
 C48(H48), C47(H47), C8(H8), C11(H11), C35(H35), C39(H39), C36(H36), C72(H72),
 C54(H54), C24(H24), C44(H44), C15(H15), C45(H45), C21(H21), C16(H16), C32(H32),
  C34(H34), C66(H66), C62(H62), C10(H10), C42(H42), C64(H64), C33(H33),
 C53(H53), C5(H5), C40(H40), C17(H17), C9(H9), C50(H50), C69(H69), C63(H63),
 C65(H65), C56(H56), C60(H60), C22(H22), C30(H30), C51(H51), C52(H52), C41(H41),
  C2(H2), C26(H26), C59(H59), C23(H23), C58(H58), C70(H70), C71(H71), C57(H57),
 C4(H4), C27(H27), C29(H29), C28(H28), C3(H3)
;
_shelx_res_checksum              50493
_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'