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_7062158
_publ_section_title
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 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         'C56 H48 Cu N2 P2, C32 H12 B F24'
_chemical_formula_sum            'C88 H60 B Cu F24 N2 P2'
_chemical_formula_weight         1737.67
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2019-09-13
_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                 95.469(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8620(12)
_cell_length_b                   19.0191(11)
_cell_length_c                   20.6755(10)
_cell_measurement_reflns_used    9585
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      2.32
_cell_volume                     7774.8(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'Bruker APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ImuS Duo Photon II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS high brilliance micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            273732
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         2.060
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0807 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.9677.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             3528
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, n-hexane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1122
_refine_ls_number_reflns         20072
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0260P)^2^+6.5432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15399
_reflns_number_total             20072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05222a2.cif
_cod_data_source_block           rd1916
_cod_depositor_comments
'Adding full bibliography for 7062150--7062158.cif.'
_cod_database_code               7062158
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.927
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F19 \\sim F20 \\sim F21 \\sim F19A \\sim F20A \\sim F21A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C44A \\sim C45A
\\sim C46A \\sim C47A \\sim C48A \\sim C49A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F19A)
\\sim Ueq, Uanis(F20A) \\sim Ueq, Uanis(F21A) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
3. Others
 Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=
 Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=1-FVAR(1)
 Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=
 Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C22(H22A,H22B), C43(H43A,H43B), C43(H43C,H43D), C50(H50A,H50B)
4.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), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A),
 C49A(H49A), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58),
 C60(H60), C62(H62), C66(H66), C68(H68), C70(H70), C74(H74), C76(H76), C78(H78),
  C82(H82), C84(H84), C86(H86)
4.c Fitted hexagon refined as free rotating group:
 C44(C45,C46,C47,C48,C49), C44A(C45A,C46A,C47A,C48A,C49A)
;
_shelx_res_checksum              96249
_olex2_submission_special_instructions 'No special instructions were received'