Developing bulky P-alkene ligands: stabilization of copper complexes with 14 valence electrons
Grasruck, Alexander; Parla, Giorgio; Heineman, Frank W.; Langer, Jens; Herrera, Alberto; Frieß, Sybille; Schmid, Günter; Dorta, Romano; New Journal of Chemistry 47 (2023) 2307–2323; doi:10.1039/D2NJ05222A

data_7062153
_publ_section_title
;
 Developing bulky P-alkene ligands: stabilization of copper complexes with
 14 valence electrons
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2307
_journal_page_last               2323
_journal_paper_doi               10.1039/D2NJ05222A
_journal_volume                  47
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C40 H48 Cl Cu N2 P2'
_chemical_formula_sum            'C40 H48 Cl Cu N2 P2'
_chemical_formula_weight         717.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-06-03 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0356(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8459(3)
_cell_length_b                   10.18035(19)
_cell_length_c                   24.1751(4)
_cell_measurement_reflns_used    32424
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      72.4120
_cell_measurement_theta_min      3.4480
_cell_volume                     3653.74(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -109.00 -16.00   1.00    1.00    --  -40.61 -38.00   0.00   93
  2  \w    -73.00 -13.00   1.00    1.00    --  -40.61 -57.00-120.00   60
  3  \w    -64.00 -18.00   1.00    1.00    --  -40.61 -38.00 -90.00   46
  4  \w   -106.00 -20.00   1.00    1.00    --  -40.61 -38.00  90.00   86
  5  \w   -115.00 -61.00   1.00    1.00    --  -40.61-153.00-125.00   54
  6  \w    -44.00 -13.00   1.00    1.00    --  -40.61 -57.00-180.00   31
  7  \w   -102.00 -46.00   1.00    1.00    --  -40.61 -57.00-180.00   56
  8  \w    -85.00  -7.00   1.00    1.00    --  -40.61 125.00 150.00   78
  9  \w    -69.00  33.00   1.00    1.00    --  -40.61  57.00 120.00  102
 10  \w   -103.00 -76.00   1.00    1.00    --  -40.61 -57.00-120.00   27
 11  \w      9.00  38.00   1.00    1.00    --   40.61  76.00-143.24   29
 12  \w      4.00  30.00   1.00    1.00    --   40.61  88.00  66.78   26
 13  \w    -29.00  34.00   1.00    1.00    --   40.61 -38.00-120.00   63
 14  \w      3.00  29.00   1.00    1.00    --   40.61  90.00-101.73   26
 15  \w     50.00  77.00   1.00    1.00    --   40.61-121.00  32.00   27
 16  \w      8.00  42.00   1.00    1.00    --   40.61  76.00 147.62   34
 17  \w     15.00  54.00   1.00    1.00    --   40.61  69.00   9.05   39
 18  \w     28.00 137.00   1.00    1.80    --  104.57 -77.00  90.00  109
 19  \w     44.00 107.00   1.00    1.80    --  104.57-111.00   0.00   63
 20  \w     75.00 101.00   1.00    1.80    --  104.57  61.00 120.00   26
 21  \w     75.00 171.00   1.00    1.80    --  104.57  61.00-180.00   96
 22  \w     75.00 101.00   1.00    1.80    --  104.57  61.00 -30.00   26
 23  \w    113.00 155.00   1.00    1.80    --  104.57  61.00 150.00   42
 24  \w    137.00 167.00   1.00    1.80    --  104.57 111.00-180.00   30
 25  \w    121.00 177.00   1.00    1.80    --  104.57  61.00 -30.00   56
 26  \w     46.00 109.00   1.00    1.80    --  104.57-111.00 -90.00   63
 27  \w     75.00 158.00   1.00    1.80    --  104.57  61.00  60.00   83
 28  \w     24.00 105.00   1.00    1.80    --  104.57 -94.00  30.00   81
 29  \w     75.00 173.00   1.00    1.80    --  104.57  61.00  30.00   98
 30  \w     75.00 101.00   1.00    1.80    --  104.57  61.00   0.00   26
 31  \w     75.00 102.00   1.00    1.80    --  104.57  61.00 150.00   27
 32  \w    119.00 176.00   1.00    1.80    --  104.57  61.00-150.00   57
 33  \w     75.00 101.00   1.00    1.80    --  104.57  61.00-150.00   26
 34  \w     80.00 105.00   1.00    1.80    --  104.57  45.00  30.00   25
 35  \w     75.00 101.00   1.00    1.80    --  104.57  61.00 -60.00   26
 36  \w     79.00 112.00   1.00    1.80    --  104.57  45.00   0.00   33
 37  \w     79.00 106.00   1.00    1.80    --  104.57  45.00 150.00   27
 38  \w    115.00 173.00   1.00    1.80    --  104.57  61.00  90.00   58
 39  \w     75.00 102.00   1.00    1.80    --  104.57  61.00-120.00   27
 40  \w     80.00 131.00   1.00    1.80    --  104.57  45.00 -30.00   51
 41  \w    107.00 132.00   1.00    1.80    --  104.57-153.00-125.00   25
 42  \w     56.00  89.00   1.00    1.80    --  104.57-153.00-125.00   33
 43  \w     75.00 108.00   1.00    1.80    --  104.57  61.00  90.00   33
 44  \w     80.00 107.00   1.00    1.80    --  104.57  45.00 -60.00   27
 45  \w     28.00  74.00   1.00    1.80    --  104.57 -94.00 -60.00   46
 46  \w     75.00 177.00   1.00    1.80    --  104.57  61.00 -90.00  102
 47  \w     79.00 158.00   1.00    1.80    --  104.57  45.00 -90.00   79
 48  \w    121.00 177.00   1.00    1.80    --  104.57  61.00   0.00   56
 49  \w    117.00 167.00   1.00    1.80    --  104.57  61.00 120.00   50
 50  \w     76.00 106.00   1.00    1.80    --  104.57  57.00-122.89   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0564502000
_diffrn_orient_matrix_UB_12      0.1204543000
_diffrn_orient_matrix_UB_13      -0.0169251000
_diffrn_orient_matrix_UB_21      0.0054302000
_diffrn_orient_matrix_UB_22      -0.0429282000
_diffrn_orient_matrix_UB_23      -0.0609990000
_diffrn_orient_matrix_UB_31      -0.0869069000
_diffrn_orient_matrix_UB_32      -0.0809820000
_diffrn_orient_matrix_UB_33      0.0071558000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53396
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.422
_diffrn_reflns_theta_min         2.977
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.368
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.506
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 6350 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         14237
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+7.0828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                14063
_reflns_number_total             14237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05222a2.cif
_cod_data_source_block           rodo211108a
_cod_depositor_comments
'Adding full bibliography for 7062150--7062158.cif.'
_cod_original_cell_volume        3653.72(12)
_cod_database_code               7062153
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H48ClCuN2P2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5112(15)
 0.4888(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C35(H35), C38(H38), C55(H55), C58(H58), C75(H75), C78(H78)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C30(H30),
  C31(H31), C32(H32), C33(H33), C42(H42), C43(H43), C44(H44), C45(H45),
 C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C62(H62), C63(H63),
  C64(H64), C65(H65), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73)
3.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C19(H19a,H19b,H19c), C20(H20a,H20b,
 H20c), C36(H36a,H36b,H36c), C37(H37a,H37b,H37c), C39(H39a,H39b,H39c), C40(H40a,
 H40b,H40c), C56(H56a,H56b,H56c), C57(H57a,H57b,H57c), C59(H59a,H59b,H59c),
 C60(H60a,H60b,H60c), C76(H76a,H76b,H76c), C77(H77a,H77b,H77c), C79(H79a,H79b,
 H79c), C80(H80a,H80b,H80c)
;
_shelx_res_checksum              48084
_olex2_date_sample_data_collection 2021-11-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.833