Exploring steric and electronic parameters of biaryl phosphacycles
Lamola, Jairus L.; Adeyinka, Adedapo S.; Malan, Frederick P.; Moshapo, Paseka T.; Holzapfel, Cedric W.; Maumela, Munaka Christopher; New Journal of Chemistry 46 (2022) 4677–4686; doi:10.1039/D1NJ05769C

data_7061287
_publ_section_title
;
 Exploring steric and electronic parameters of biaryl phosphacycles
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4677
_journal_page_last               4686
_journal_paper_doi               10.1039/D1NJ05769C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C22 H25 O3 P Se'
_chemical_formula_sum            'C22 H25 O3 P Se'
_chemical_formula_weight         447.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-11-06
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-12-22 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.67870(10)
_cell_length_b                   13.38680(10)
_cell_length_c                   16.7162(2)
_cell_measurement_reflns_used    25352
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      76.0430
_cell_measurement_theta_min      2.7240
_cell_volume                     2107.29(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00  60.00   64
  2  \w    -24.00  74.00   0.50    0.05    --   47.20 -87.00 178.00  196
  3  \w     32.00 132.00   0.50    0.05    --  104.75 -87.00 178.00  200
  4  \w     92.00 178.00   0.50    0.05    --  104.75  30.00  60.00  172
  5  \w     84.00 178.00   0.50    0.05    --  104.75  87.00 -64.00  188
  6  \w     88.00 178.00   0.50    0.05    --  104.75  61.00  30.00  180
  7  \w     32.00  80.00   0.50    0.05    --  104.75 -61.00-180.00   96
  8  \w     32.00  80.00   0.50    0.05    --  104.75 -61.00-150.00   96
  9  \w     32.00 128.00   0.50    0.05    --  104.75 -77.00-180.00  192
 10  \w     32.00  80.00   0.50    0.05    --  104.75 -61.00 -30.00   96
 11  \w     32.00 112.00   0.50    0.05    --  104.75-125.00  30.00  160
 12  \w     32.00 106.00   0.50    0.05    --  104.75 -94.00 120.00  148
 13  \w     32.00 106.00   0.50    0.05    --  104.75 -94.00  90.00  148
 14  \w     32.00 106.00   0.50    0.05    --  104.75 -94.00-120.00  148
 15  \w    -27.00  12.00   0.50    0.05    --   47.20 -19.00 -90.00   78
 16  \w    -27.00  12.00   0.50    0.05    --   47.20 -19.00-120.00   78
 17  \w    -27.00  12.00   0.50    0.05    --   47.20 -19.00-180.00   78
 18  \w    -74.00  26.00   0.50    0.05    --  -47.20  87.00 -64.00  200
 19  \w    -27.00  12.00   0.50    0.05    --   47.20 -19.00  60.00   78
 20  \w   -120.00 -74.00   0.50    0.05    --  -47.20-125.00 -90.00   92
 21  \w   -120.00 -24.00   0.50    0.05    --  -47.20 -77.00 -60.00  192
 22  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00   0.00   86
 23  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00 -60.00   86
 24  \w   -120.00 -32.00   0.50    0.05    --  -47.20 -57.00 -30.00  176
 25  \w   -120.00 -24.00   0.50    0.05    --  -47.20 -77.00  60.00  192
 26  \w   -120.00 -32.00   0.50    0.05    --  -47.20 -57.00-150.00  176
 27  \w   -120.00 -24.00   0.50    0.05    --  -47.20 -77.00-180.00  192
 28  \w   -129.00 -29.00   0.50    0.05    -- -102.00  87.00 -64.00  200
 29  \w   -175.00 -80.00   0.50    0.05    -- -102.00 -87.00 178.00  190
 30  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -77.00 150.00  192
 31  \w   -174.00 -89.00   0.50    0.05    -- -102.00 -45.00  30.00  170
 32  \w   -174.00 -89.00   0.50    0.05    -- -102.00 -45.00-120.00  170
 33  \w   -175.00 -85.00   0.50    0.05    -- -102.00 -61.00 -60.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0750699000
_diffrn_orient_matrix_UB_12      -0.0566612000
_diffrn_orient_matrix_UB_13      -0.0581065000
_diffrn_orient_matrix_UB_21      0.0344016000
_diffrn_orient_matrix_UB_22      -0.0861049000
_diffrn_orient_matrix_UB_23      0.0626721000
_diffrn_orient_matrix_UB_31      -0.1411187000
_diffrn_orient_matrix_UB_32      -0.0511215000
_diffrn_orient_matrix_UB_33      -0.0410128000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28024
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.253
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.294
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0379P)^2^+1.3893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4231
_reflns_number_total             4321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj05_lt
_cod_depositor_comments
'Adding full bibliography for 7061279--7061288.cif.'
_cod_database_code               7061287
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N O P Se'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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:
 C4(H4A,H4B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C9(H9), C10(H10), C18(H18), C8(H8), C17(H17), C15(H15),
 C16(H16)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              91526
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.523
_oxdiff_exptl_absorpt_empirical_full_min 0.327