Unusual coordination mode for 1,3-diphosphete ligands towards a Cr-Cr quintuple bond complex.
Elsayed Moussa, M.; Rummel, E.-M.; Balázs, G; Riesinger, C.; Noor, A.; Kempe, R.; Scheer, M.; Chemical communications (Cambridge, England) 59 (2023) 8588–8591; doi:10.1039/d3cc01358h

data_7131853
_publ_section_title
;
 Unusual coordination mode for 1,3-diphosphete ligands towards a Cr-Cr
 quintuple bond complex.
;
_journal_issue                   55
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8588
_journal_page_last               8591
_journal_paper_doi               10.1039/d3cc01358h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C61 H73 Cr2 N4 P'
_chemical_formula_sum            'C61 H73 Cr2 N4 P'
_chemical_formula_weight         997.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-26
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-03-08 deposited with the CCDC.	2023-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.268(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2784(6)
_cell_length_b                   22.2038(13)
_cell_length_c                   12.5344(5)
_cell_measurement_reflns_used    2952
_cell_measurement_temperature    123.1(3)
_cell_measurement_theta_max      73.8060
_cell_measurement_theta_min      4.1390
_cell_volume                     2759.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.1
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
  1 omega   41.00  118.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.5756 -178.0000    0.0000 154

  2 omega   18.00  111.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       43.5756   77.0000   90.0000 186

  3 omega   33.00  120.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   30.0000 174

  4 omega   96.00  172.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  150.0000 152

  5 omega   33.00   91.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -30.0000 116

  6 omega   39.00  124.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000   30.0000 170

  7 omega   32.00   83.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   30.0000 102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9570
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.377
_diffrn_reflns_theta_min         4.163
_exptl_absorpt_coefficient_mu    3.820
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       plate
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.1008
_exptl_crystal_size_mid          0.0728
_exptl_crystal_size_min          0.0211
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1539P)^2^+1.4619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2358
_refine_ls_wR_factor_ref         0.2465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3731
_reflns_number_total             5342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01358h2.cif
_cod_data_source_block           mp_abs
_cod_database_code               7131853
_shelx_shelxl_version_number     2018/3
_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: C1(0.5) P1(0.5) C2(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) C9(0.5) H9(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5)
 H11A(0.5) H11B(0.5)
3.a Ternary CH refined with riding coordinates:
 C31(H31), C34(H34), C4(H4), C6(H6), C9(H9)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,
 H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C27(H27),
 C28(H28), C29(H29)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              51680
_shelx_hkl_checksum              45971
_olex2_submission_special_instructions 'No special instructions were received'