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_7131852
_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         'C60 H76 Cr2 N4 P2, C6 H14'
_chemical_formula_sum            'C66 H90 Cr2 N4 P2'
_chemical_formula_weight         1105.35
_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
_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                99.9375(13)
_cell_angle_beta                 90.7104(13)
_cell_angle_gamma                92.7071(12)
_cell_formula_units_Z            2
_cell_length_a                   12.8677(2)
_cell_length_b                   13.10453(19)
_cell_length_c                   18.2132(3)
_cell_measurement_reflns_used    26441
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.7605
_cell_measurement_theta_min      3.4283
_cell_volume                     3021.09(8)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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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      123.01
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -70.00   33.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   57.0000  -30.0000 206

  2 omega  -71.00   37.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   77.0000   60.0000 216

  3 omega  -11.00   19.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   57.0000 -150.0000 60

  4 omega  -71.00  -44.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814   57.0000 -150.0000 54

  5 omega    7.00  102.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.0814   77.0000 -180.0000 190

  6 omega    5.00   35.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.0814 -125.0000  120.0000 60

  7 omega   29.00   68.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  120.0000 78

  8 omega   33.00   59.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   60.0000 52

  9 omega   35.00  140.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000 -150.0000 210

 10 omega   37.00   69.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -120.0000 64

 11 omega   31.00   69.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000    0.0000 76

 12 omega   84.00  117.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   30.0000 66

 13 omega   99.00  156.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000   30.0000 114

 14 omega   62.00  150.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   15.0000  150.0000 176

 15 omega   54.00  120.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000 -150.0000 132

 16 omega   33.00  141.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000    0.0000 216

 17 omega   30.00   56.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  150.0000 52

 18 omega   42.00   69.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -150.0000 54

 19 omega   31.00   58.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   90.0000 54

 20 omega   80.00  134.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000    0.0000 108

 21 omega   79.00  112.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -90.0000 66

 22 omega -115.00  -11.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000  -30.0000 208

 23 omega -115.00  -11.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -57.0000   60.0000 208

 24 omega -117.00  -15.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -37.0000   90.0000 204

 25 omega -120.00   -7.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -77.0000  -30.0000 226

 26 omega  -98.00   -2.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  125.0000   90.0000 192

 27 omega -120.00   -7.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -77.0000 -120.0000 226

 28 omega -162.00 -132.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000 -180.0000 60

 29 omega -162.00  -49.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000    0.0000 226

 30 omega -162.00  -49.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000   90.0000 226

 31 omega   77.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -180.0000 162

 32 omega   73.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  120.0000 170

 33 omega   79.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -120.0000 158

 34 omega   23.00  109.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  120.0000 172

 35 omega   32.00   77.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  -60.0000 90

 36 omega   77.00   87.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   60.0000 20
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.761
_diffrn_reflns_theta_min         3.428
_exptl_absorpt_coefficient_mu    3.776
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.571
_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_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2143
_exptl_crystal_size_mid          0.1185
_exptl_crystal_size_min          0.0946
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         11915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0429P)^2^+1.9196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11037
_reflns_number_total             11915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01358h2.cif
_cod_data_source_block           ap_abs
_cod_database_code               7131852
_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.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C55(H55), C58(H58)
2.b Secondary CH2 refined with riding coordinates:
 C101(H10G,H10H), C102(H10I,H10J), C103(H10K,H10L), C104(H10M,H10N)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C18(H18), C19(H19), C20(H20), C26(H26),
 C27(H27), C28(H28), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C45(H45),
  C51(H51), C52(H52), C53(H53)
2.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C100(H10D,H10E,H10F),
 C105(H10O,H10P,H10Q)
;
_shelx_res_checksum              75360
_shelx_hkl_checksum              81616
_olex2_submission_special_instructions 'No special instructions were received'