Ultrafast electronic, infrared, and X-ray absorption spectroscopy study of Cu(I) phosphine diimine complexes.
Appleby, Martin V.; Cowin, Rory A.; Ivalo, Iona I.; Peralta-Arriaga, Samantha L; Robertson, Craig C.; Bartlett, Stuart; Fitzpatrick, Ann; Dent, Andrew; Karras, Gabriel; Diaz-Moreno, Sofia; Chekulaev, Dimitri; Weinstein, Julia A.; Faraday discussions 244 (2023) 391–410; doi:10.1039/d3fd00027c

data_1569482
_publ_section_title
;
 Ultrafast electronic, infrared, and X-ray absorption spectroscopy study
 of Cu(I) phosphine diimine complexes.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              391
_journal_page_last               410
_journal_paper_doi               10.1039/d3fd00027c
_journal_volume                  244
_journal_year                    2023
_chemical_formula_moiety         'C60 H48 Cu N2 O5 P2, B F4'
_chemical_formula_sum            'C60 H48 B Cu F4 N2 O5 P2'
_chemical_formula_weight         1089.29
_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             2023-02-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-02 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.722(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2437(18)
_cell_length_b                   10.7278(10)
_cell_length_c                   29.075(3)
_cell_measurement_reflns_used    3384
_cell_measurement_temperature    100
_cell_measurement_theta_max      18.646
_cell_measurement_theta_min      2.885
_cell_volume                     5225.0(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1572
_diffrn_reflns_av_unetI/netI     0.2010
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            45782
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.654
_diffrn_reflns_theta_min         2.453
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.7307.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         11928
_refine_ls_number_restraints     762
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.2138
_refine_ls_R_factor_gt           0.0931
_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^)+(0.0879P)^2^+15.0924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5597
_reflns_number_total             11928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3fd00027c2.cif
_cod_data_source_block           ch1jw310k_0m
_cod_depositor_comments
'Adding full bibliography for 1569481--1569483.cif.'
_cod_original_cell_volume        5224.9(9)
_cod_database_code               1569482
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.799
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H7A)=Sof(O1B)=Sof(C16B)=Sof(H16B)=Sof(C15B)=Sof(H15B)=Sof(C14B)=Sof(H14B)=
 Sof(C17B)=Sof(H17B)=Sof(C19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24B)=Sof(C13B)=
 Sof(C18B)=Sof(H18B)=Sof(C6B)=Sof(C5B)=Sof(H5B)=Sof(C4B)=Sof(H4B)=Sof(C3B)=
 Sof(H3B)=Sof(C2B)=Sof(H2B)=Sof(C1B)=1-FVAR(1)
 Sof(H7B)=Sof(O1A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C13A)=Sof(C17A)=
 Sof(H17A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C1A)=Sof(C6A)=Sof(C5A)=
 Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=Sof(C2A)=Sof(H2A)=Sof(C18A)=
 Sof(H18A)=Sof(C14A)=Sof(H14A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C56(H56A,H56B)
4.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C53(H53), C36(H36), C38(H38), C50(H50), C40(H40), C44(H44),
 C33(H33), C7A(H7A), C35(H35), C8A(H8A), C9A(H9A), C39(H39), C10A(H10A),
 C41(H41), C11A(H11A), C47(H47), C7B(H7B), C8B(H8B), C52(H52), C9B(H9B),
 C10B(H10B), C11B(H11B), C32(H32), C51(H51), C16B(H16B), C15B(H15B), C14B(H14B),
  C17B(H17B), C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B),
 C18B(H18B), C5B(H5B), C4B(H4B), C3B(H3B), C2B(H2B), C16A(H16A), C15A(H15A),
 C17A(H17A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A),
 C5A(H5A), C4A(H4A), C3A(H3A), C2A(H2A), C18A(H18A), C14A(H14A)
4.c Fitted hexagon refined as free rotating group:
 C19B(C20B,C21B,C22B,C23B,C24B), C6B(C5B,C4B,C3B,C2B,C1B), C19A(C20A,C21A,C22A,
 C23A,C24A), C1A(C6A,C5A,C4A,C3A,C2A)
4.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              29195
_olex2_exptl_crystal_mounting_method 'mitigen microloop in fomblin oil'
_olex2_submission_original_sample_id 'Cu DPEPhos DCBQ BF4'
_olex2_submission_special_instructions 'No special instructions were received'