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_7062156
_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         'C42 H30 Cl Cu N3 P, 3(C H2 Cl2)'
_chemical_formula_sum            'C45 H36 Cl7 Cu N3 P'
_chemical_formula_weight         961.43
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-24 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.171(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5083(5)
_cell_length_b                   24.4621(11)
_cell_length_c                   16.5527(7)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.33
_cell_volume                     4221.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            130122
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.673
_diffrn_reflns_theta_min         1.493
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0482 before and 0.0391 after correction.
The Ratio of minimum to maximum transmission is 0.8897.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, n-pentane'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         11774
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0362P)^2^+4.5147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9900
_reflns_number_total             11774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05222a2.cif
_cod_data_source_block           rd1726
_cod_depositor_comments
'Adding full bibliography for 7062150--7062158.cif.'
_cod_database_code               7062156
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.676
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C300 \\sim Cl31 \\sim Cl32 \\sim C310 \\sim Cl33 \\sim Cl34: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C300) \\sim Ueq, Uanis(Cl31) \\sim Ueq, Uanis(Cl32) \\sim Ueq,
Uanis(C310) \\sim Ueq, Uanis(Cl33) \\sim Ueq, Uanis(Cl34) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Same fragment restrains
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C300, Cl31, Cl32}
{C100, Cl11, Cl12} sigma for 1-2: 0.02, 1-3: 0.04
as
{C310, Cl33, Cl34}
4. Others
 Sof(C310)=Sof(H31A)=Sof(H31B)=Sof(Cl33)=Sof(Cl34)=1-FVAR(1)
 Sof(C300)=Sof(H30A)=Sof(H30B)=Sof(Cl31)=Sof(Cl32)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C200(H20A,H20B), C300(H30A,H30B), C310(H31A,H31B)
5.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), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_res_checksum              7898
_olex2_submission_special_instructions 'No special instructions were received'