Electrostatic vs. Inductive Effects in Phosphine Ligand Donor Properties and Reactivity
Kelty, Margaret L.; McNeece, Andrew J.; Kurutz, Josh W.; Filatov, Alexander S.; Anderson, John S.; Chemical Science  (2022) –; doi:10.1039/D1SC04277G

data_1566620
_publ_section_title
;
 Electrostatic vs. Inductive Effects in Phosphine Ligand Donor Properties
 and Reactivity
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04277G
_journal_year                    2022
_chemical_formula_moiety         'C19 H19 B F3 O3 P Rh, C24 H20 P'
_chemical_formula_sum            'C43 H39 B F3 O3 P2 Rh'
_chemical_formula_weight         836.40
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-16 deposited with the CCDC.	2022-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                83.172(2)
_cell_angle_beta                 88.634(2)
_cell_angle_gamma                79.181(2)
_cell_formula_units_Z            4
_cell_length_a                   9.1533(6)
_cell_length_b                   13.0253(9)
_cell_length_c                   33.273(2)
_cell_measurement_reflns_used    8310
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.30
_cell_volume                     3868.8(4)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2018/1 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  D8Venture
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43102
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        24.149
_diffrn_reflns_theta_max         24.149
_diffrn_reflns_theta_min         2.265
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1158 before and 0.0549 after correction. 
The Ratio of minimum to maximum transmission is 0.9039.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         12044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0424
_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^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8452
_reflns_number_total             12044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04277g2.cif
_cod_data_source_block           mo_0906_am_0m
_cod_database_code               1566620
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.773
_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.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
  C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67),
  C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76),
 C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84), C85(H85),
  C86(H86)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              60565
_olex2_submission_special_instructions 'No special instructions were received'