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_1566619
_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         'C18 H14 B F3 P Se, C24 H20 P'
_chemical_formula_sum            'C42 H34 B F3 P2 Se'
_chemical_formula_weight         747.40
_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             2020-09-01
_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                84.9610(10)
_cell_angle_beta                 77.687(2)
_cell_angle_gamma                74.085(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6724(5)
_cell_length_b                   12.8821(6)
_cell_length_c                   14.5407(7)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.22
_cell_volume                     1701.43(15)
_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-2018/3 (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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62543
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.379
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0908 before and 0.0435 after correction. The Ratio of minimum to maximum transmission is 0.8998. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0327P)^2^+1.2298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7613
_reflns_number_total             8501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04277g2.cif
_cod_data_source_block           try1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'difference map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1566619
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.704
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.017) H3(0.02) H4(0.023) H5(0.018) H8(0.022) H9(0.029)
 H10(0.031) H11(0.03) H12(0.023) H14(0.018) H15(0.021) H16(0.023) H17(0.023)
 H18(0.018) H20(0.018) H21(0.022) H22(0.022) H23(0.02) H24(0.016) H26(0.016)
 H27(0.019) H28(0.02) H29(0.018) H30(0.016) H32(0.02) H33(0.024) H34(0.021)
 H35(0.019) H36(0.017) H38(0.017) H39(0.022) H40(0.023) H41(0.022) H42(0.019)
 Fixed X: H2(0.84379) H3(1.096098) H4(1.215917) H5(1.080252) H8(0.900367)
 H9(1.087807) H10(1.241213) H11(1.199348) H12(1.007782) H14(0.696133)
 H15(0.500485) H16(0.336278) H17(0.367009) H18(0.559898) H20(0.784924)
 H21(0.659434) H22(0.538371) H23(0.543662) H24(0.67153) H26(0.683867)
 H27(0.580606) H28(0.58522) H29(0.69333) H30(0.808063) H32(1.039561)
 H33(1.278139) H34(1.398781) H35(1.28428) H36(1.049447) H38(1.059311)
 H39(1.049449) H40(0.830228) H41(0.617586) H42(0.625265)
 Fixed Y: H2(0.093019) H3(0.061681) H4(0.125032) H5(0.209889) H8(0.09359)
 H9(0.035091) H10(0.144753) H11(0.316682) H12(0.378531) H14(0.086446)
 H15(0.032675) H16(0.148254) H17(0.318676) H18(0.375343) H20(0.236642)
 H21(0.107572) H22(0.036845) H23(0.093416) H24(0.220342) H26(0.559662)
 H27(0.670404) H28(0.597736) H29(0.414073) H30(0.304427) H32(0.143223)
 H33(0.047289) H34(0.105621) H35(0.260892) H36(0.362188) H38(0.421153)
 H39(0.542449) H40(0.613658) H41(0.566316) H42(0.444171)
 Fixed Z: H2(0.379578) H3(0.349353) H4(0.206825) H5(0.094133) H8(-0.037396)
 H9(-0.167372) H10(-0.234868) H11(-0.178455) H12(-0.051103) H14(0.113949)
 H15(0.081272) H16(-0.002753) H17(-0.054283) H18(-0.019384) H20(0.782205)
 H21(0.846801) H22(0.755134) H23(0.597726) H24(0.53101) H26(0.584878)
 H27(0.467554) H28(0.324999) H29(0.298764) H30(0.412078) H32(0.648034)
 H33(0.582733) H34(0.439304) H35(0.361366) H36(0.429053) H38(0.651477)
 H39(0.765385) H40(0.868467) H41(0.859521) H42(0.747691)
;
_shelx_res_checksum              77466
_olex2_submission_special_instructions 'No special instructions were received'