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_1568807
_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         'C34 H43 N3 P Rh'
_chemical_formula_sum            'C34 H43 N3 P Rh'
_chemical_formula_weight         627.59
_chemical_name_systematic
;
 [(NDipp)2(CMe)2(C5H3N)]Rh(CP)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 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            4
_cell_length_a                   8.49660(10)
_cell_length_b                   17.9973(2)
_cell_length_c                   20.3635(2)
_cell_measurement_reflns_used    40301
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.2750
_cell_measurement_theta_min      4.2450
_cell_volume                     3113.90(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64682
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.183
_diffrn_reflns_theta_min         4.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       needle
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 2689 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0360P)^2^+0.7976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6310
_reflns_number_total             6499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01126g3.cif
_cod_data_source_block           ESY175
_cod_depositor_comments
'Adding full bibliography for 1568803--1568814.cif.'
_cod_database_code               1568807
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.905
_shelx_res_checksum              65337
_shelx_hkl_checksum              96268