Putting cyaphide in its place: determining the donor/acceptor properties of the κC-cyaphido ligand
Yang, Eric S.; Combey, Emma; Goicoechea, Jose M.; Chemical Science 14 (2023) 4627–4632; doi:10.1039/D3SC01126G

data_1568814
_publ_section_title
;
 Putting cyaphide in its place: determining the donor/acceptor properties
 of the \kC-cyaphido ligand
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              4627
_journal_page_last               4632
_journal_paper_doi               10.1039/D3SC01126G
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C33 H43 Cl N3 Rh, 1.333(C4 H8 O),0.666(C5 H12)'
_chemical_formula_sum            'C41.666 H61.666 Cl N3 O1.333 Rh'
_chemical_formula_weight         764.30
_chemical_name_systematic
;
 {(NDipp)2(CMe)2(C5H3N)}RhCl*1.333THF*0.666pent
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   17.36740(10)
_cell_length_b                   29.7047(2)
_cell_length_c                   23.95240(10)
_cell_measurement_reflns_used    44115
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.1710
_cell_measurement_theta_min      3.4380
_cell_volume                     12356.89(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SUPERFLIP (Palatinus and Chapuis, 2007)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            102303
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.291
_diffrn_reflns_theta_min         2.947
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       plate
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.657
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 5359 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         12891
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0599P)^2^+14.4201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                12153
_reflns_number_total             12891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01126g3.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1568803--1568814.cif.'
_cod_original_cell_volume        12356.88(12)
_cod_database_code               1568814
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.487
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              63136
_shelx_hkl_checksum              31238