Non-spectator behavior of a neutral phosphine ligand driven by a redox-active boron cluster.
Riffle, Jared R.; Jowers, Cash L.; Luna, Sarah; Smith, Mark D.; Peryshkov, Dmitry V.; Chemical science 16 (2025) 15997–16003; doi:10.1039/d5sc04058b

data_1575270
_publ_section_title
;
 Non-spectator behavior of a neutral phosphine ligand driven by a
 redox-active boron cluster.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              15997
_journal_page_last               16003
_journal_paper_doi               10.1039/d5sc04058b
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C26 H61 B20 Cl Cu P3, C4 H8 O'
_chemical_formula_sum            'C30 H69 B20 Cl Cu O P3'
_chemical_formula_weight         853.95
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-05-23 deposited with the CCDC.	2025-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                77.677(2)
_cell_angle_beta                 84.292(2)
_cell_angle_gamma                77.488(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3745(4)
_cell_length_b                   10.5931(5)
_cell_length_c                   21.3748(9)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.566
_cell_measurement_theta_min      2.401
_cell_volume                     2236.93(17)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker APEX3 v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 PHOTON-II
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            108509
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.589
_diffrn_reflns_theta_min         2.053
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.5650
_exptl_absorpt_correction_T_min  0.4812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1202 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.8517.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         14830
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.8950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12675
_reflns_number_total             14830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04058b2.cif
_cod_data_source_block           jrxr_03_97
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1575269--1575273.cif.
;
_cod_database_code               1575270
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.853
_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. Uiso/Uaniso restraints and constraints
Uanis(C3S) = Uanis(C5S)
Uanis(C2S) = Uanis(C6S)
Uanis(C1S) = Uanis(C7S)
Uanis(O1S) = Uanis(C8S)
Uanis(C4S) = Uanis(O2S)
3. Same fragment restrains
{O1S, C1S, C2S, C3S, C4S} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O2S, C5S, C6S, C7S, C8S}
4. Others
 Sof(O2S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(C7S)=
 Sof(H7SA)=Sof(H7SB)=Sof(C8S)=Sof(H8SA)=Sof(H8SB)=1-FVAR(1)
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,
 H5SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB), C8S(H8SA,H8SB)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12A), C13(H13A), C14(H14A), C15(H15A), C16(H16A)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              75028
_olex2_submission_special_instructions 'No special instructions were received'