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_1569483
_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
'C63 H52 Cu N2 O5 P2, 0.533(B F4), 0.467(B F3), 0.467(F)'
_chemical_formula_sum            'C63 H52 B Cu F4 N2 O5 P2'
_chemical_formula_weight         1129.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-04 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                73.672(3)
_cell_angle_beta                 86.086(3)
_cell_angle_gamma                70.147(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2410(5)
_cell_length_b                   14.6532(8)
_cell_length_c                   18.4225(8)
_cell_measurement_reflns_used    7627
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      69.737
_cell_measurement_theta_min      3.335
_cell_volume                     2737.8(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker D8 Venture Photon III'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57710
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.817
_diffrn_reflns_theta_min         2.500
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1168 before and 0.0829 after correction.
The Ratio of minimum to maximum transmission is 0.7137.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.105
_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     906
_refine_ls_number_reflns         10363
_refine_ls_number_restraints     860
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0972
_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^)+(0.1440P)^2^+9.8274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2549
_refine_ls_wR_factor_ref         0.3025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6737
_reflns_number_total             10363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3fd00027c2.cif
_cod_data_source_block           ch1jw309v_0m
_cod_depositor_comments
'Adding full bibliography for 1569481--1569483.cif.'
_cod_database_code               1569483
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.700
_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. Restrained distances
 C63A-C62A \\sim C62B-C63B
 with sigma of 0.02
 O4B-C51B \\sim O4A-C51A
 with sigma of 0.02
 N2-C57A \\sim N2-C57B
 with sigma of 0.02
 O5B-C62B \\sim O5A-C62A
 with sigma of 0.02
 N2-C49A \\sim N2-C49B
 with sigma of 0.02
 C57A-C56A \\sim C57B-C56B
 with sigma of 0.02
 C48-C50A \\sim C48-C50B
 with sigma of 0.04
 C57A-C52A \\sim C57B-C52B
 with sigma of 0.02
 C52A-C50A \\sim C52B-C50B
 with sigma of 0.04
 C48-C49A \\sim C48-C49B
 with sigma of 0.02
 C54A-C55A \\sim C54B-C55B
 with sigma of 0.02
 C57A-C51A \\sim C57B-C51B
 with sigma of 0.04
 C54A-C52A \\sim C54B-C52B
 with sigma of 0.04
 C49A-C50A \\sim C49B-C50B
 with sigma of 0.02
 C55A-C53A \\sim C55B-C53B
 with sigma of 0.04
 C55A-C56A \\sim C55B-C56B
 with sigma of 0.02
 C53A-C51A \\sim C53B-C51B
 with sigma of 0.04
 C52A-C53A \\sim C52B-C53B
 with sigma of 0.02
 C52A-C51A \\sim C52B-C51B
 with sigma of 0.02
 C54A-C53A \\sim C54B-C53B
 with sigma of 0.02
 C54A-C56A \\sim C54B-C56B
 with sigma of 0.04
 C49A-C51A \\sim C49B-C51B
 with sigma of 0.04
 C56A-C52A \\sim C56B-C52B
 with sigma of 0.04
 N2-C56A \\sim N2-C56B
 with sigma of 0.04
 N2-C52A \\sim N2-C52B
 with sigma of 0.04
 N2-C50A \\sim N2-C50B
 with sigma of 0.04
 C57A-C55A \\sim C57B-C55B
 with sigma of 0.04
 C50A-C51A \\sim C50B-C51B
 with sigma of 0.02
 C57A-C53A \\sim C57B-C53B
 with sigma of 0.04
 C61B-C51B \\sim C61A-C51A
 with sigma of 0.02
 O4B-C61B \\sim O4A-C61A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4B) = Uanis(C61B) = Uanis(O5B) = Uanis(C62B) = Uanis(C63B)
Uanis(C61B) = Uanis(O5B) = Uanis(C62B) = Uanis(C63B)
4. 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
5. Others
 Sof(C34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=Sof(H37B)=
 Sof(C38B)=Sof(H38B)=Sof(C39B)=Sof(H39B)=1-FVAR(1)
 Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=
 Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=FVAR(1)
 Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=
 Sof(H26B)=Sof(C27B)=Sof(H27B)=1-FVAR(2)
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=
 Sof(H26A)=Sof(C27A)=Sof(H27A)=FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(O4B)=Sof(O5B)=Sof(C49B)=Sof(C50B)=
 Sof(H50B)=Sof(C51B)=Sof(C52B)=Sof(C53B)=Sof(H53B)=Sof(C54B)=Sof(H54B)=
 Sof(C55B)=Sof(H55B)=Sof(C56B)=Sof(H56B)=Sof(C57B)=Sof(C61B)=Sof(C62B)=
 Sof(H62A)=Sof(H62B)=Sof(C63B)=Sof(H63C)=Sof(H63A)=Sof(H63B)=Sof(B1B)=1-FVAR(3)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(O4A)=Sof(O5A)=Sof(C49A)=Sof(C50A)=
 Sof(H50A)=Sof(C51A)=Sof(C52A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(C61A)=Sof(C62A)=
 Sof(H62C)=Sof(H62D)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(B1A)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C62A(H62C,H62D), C62B(H62A,H62B)
6.b Me refined with riding coordinates:
 C63B(H63C,H63A,H63B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C41(H41), C42(H42), C43(H43), C44(H44), C47(H47), C23A(H23A), C24A(H24A),
 C25A(H25A), C26A(H26A), C27A(H27A), C35A(H35A), C36A(H36A), C37A(H37A),
 C38A(H38A), C39A(H39A), C50A(H50A), C53A(H53A), C54A(H54A), C55A(H55A),
 C56A(H56A), C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B),
 C35B(H35B), C36B(H36B), C37B(H37B), C38B(H38B), C39B(H39B), C50B(H50B),
 C53B(H53B), C54B(H54B), C55B(H55B), C56B(H56B)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C60(H60A,H60B,H60C), C63A(H63D,H63E,
 H63F)
;
_shelx_res_checksum              6061
_olex2_submission_special_instructions 'No special instructions were received'