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_7062152
_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_formula_moiety         'C70 H54 Cl2 Cu2 N4 P2'
_chemical_formula_sum            'C70 H54 Cl2 Cu2 N4 P2'
_chemical_formula_weight         1211.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-30 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.629(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9046(2)
_cell_length_b                   20.3977(3)
_cell_length_c                   14.4741(2)
_cell_measurement_reflns_used    6760
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.5180
_cell_measurement_theta_min      3.1410
_cell_volume                     2786.89(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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    -87.00  -8.00   1.00    1.50    --  -41.15 125.00   0.00   79
  2  \w    -40.00 -13.00   1.00    1.50    --  -41.15 125.00 -90.00   27
  3  \w   -112.00 -17.00   1.00    1.50    --  -41.15 -38.00  60.00   95
  4  \w     35.00 122.00   1.00    2.00    --  104.35 -61.00-120.00   87
  5  \w     69.00 106.00   1.00    2.00    --  104.35 -94.00  90.00   37
  6  \w     22.00  52.00   1.00    2.00    --  104.35 -94.00  90.00   30
  7  \w     76.00 156.00   1.00    2.00    --  104.35  61.00 150.00   80
  8  \w     22.00 106.00   1.00    2.00    --  104.35 -94.00-150.00   84
  9  \w     88.00 172.00   1.00    2.00    --  104.35  61.00  30.00   84
;
_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      0.0771265000
_diffrn_orient_matrix_UB_12      -0.0303474000
_diffrn_orient_matrix_UB_13      0.0994732000
_diffrn_orient_matrix_UB_21      0.1430605000
_diffrn_orient_matrix_UB_22      0.0234446000
_diffrn_orient_matrix_UB_23      -0.0095478000
_diffrn_orient_matrix_UB_31      -0.0155973000
_diffrn_orient_matrix_UB_32      0.0651405000
_diffrn_orient_matrix_UB_33      0.0496179000
_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  0.0195
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10234
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.492
_diffrn_reflns_theta_min         3.868
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.741
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0386P)^2^+1.0784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4884
_reflns_number_total             5345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05222a2.cif
_cod_data_source_block           rodo220629a
_cod_depositor_comments
'Adding full bibliography for 7062150--7062158.cif.'
_cod_original_cell_volume        2786.89(8)
_cod_database_code               7062152
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C70H54Cl2Cu2N4P2
_shelx_estimated_absorpt_t_max   0.654
_shelx_estimated_absorpt_t_min   0.534
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C9(H9), C20(H20), C34(H34), C28(H28), C5(H5), C24(H24),
 C6(H6), C14(H14), C33(H33), C25(H25), C29(H29), C3(H3), C15(H15), C11(H11),
 C7(H7), C10(H10), C12(H12), C4(H4), C17(H17), C19(H19), C18(H18), C31(H31),
 C32(H32)
;
_shelx_res_checksum              78379
_olex2_date_sample_data_collection 2022-06-29
_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 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.774