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_7061280
_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 H27 O2 P Se'
_chemical_formula_sum            'C22 H27 O2 P Se'
_chemical_formula_weight         433.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-22
_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                 90.347(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4669(2)
_cell_length_b                   17.7087(4)
_cell_length_c                   15.2071(3)
_cell_measurement_reflns_used    10869
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      75.7950
_cell_measurement_theta_min      3.8010
_cell_volume                     2010.78(8)
_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 0.958
_diffrn_measured_fraction_theta_max 0.907
_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     25.00 120.00   0.50    0.07    --   47.20  77.00  60.00  190
  2  \w     34.00 120.00   0.50    0.07    --   47.20  48.00 -43.00  172
  3  \w     91.00 176.00   0.50    0.30    --  104.75  15.00-120.00  170
  4  \w     32.00 120.00   0.50    0.07    --   47.20  57.00-180.00  176
  5  \w    -27.00  12.00   0.50    0.07    --   47.20 -19.00-150.00   78
  6  \w    -27.00  12.00   0.50    0.07    --   47.20 -19.00  30.00   78
  7  \w    -27.00  12.00   0.50    0.07    --   47.20 -19.00 -30.00   78
  8  \w     32.00  80.00   0.50    0.30    --  104.75 -61.00-120.00   96
  9  \w     32.00 128.00   0.50    0.30    --  104.75 -77.00 -30.00  192
 10  \w     32.00  80.00   0.50    0.30    --  104.75 -61.00 -30.00   96
 11  \w     -4.00  28.00   0.50    0.07    --  -47.20  19.00  60.00   64
 12  \w    -72.00 -29.00   0.50    0.30    -- -102.00  61.00 120.00   86
 13  \w    -72.00 -29.00   0.50    0.30    -- -102.00  61.00-180.00   86
 14  \w   -112.00 -29.00   0.50    0.30    -- -102.00 125.00-180.00  166
 15  \w     18.00  95.00   0.50    0.07    --   47.20-125.00 -60.00  154
 16  \w     32.00 106.00   0.50    0.30    --  104.75 -96.00 -50.00  148
 17  \w     -4.00  28.00   0.50    0.07    --  -47.20  19.00 150.00   64
 18  \w   -168.00 -90.00   0.50    0.30    -- -102.00 -15.00  60.00  156
 19  \w   -174.00 -88.00   0.50    0.30    -- -102.00 -48.00 168.00  172
 20  \w   -175.00 -80.00   0.50    0.30    -- -102.00 -84.00  45.00  190
 21  \w   -120.00 -74.00   0.50    0.07    --  -47.20-125.00 -90.00   92
;
_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      -0.1930137000
_diffrn_orient_matrix_UB_12      -0.0191557000
_diffrn_orient_matrix_UB_13      -0.0287117000
_diffrn_orient_matrix_UB_21      -0.0085761000
_diffrn_orient_matrix_UB_22      0.0736686000
_diffrn_orient_matrix_UB_23      -0.0536478000
_diffrn_orient_matrix_UB_31      0.0727158000
_diffrn_orient_matrix_UB_32      -0.0420186000
_diffrn_orient_matrix_UB_33      -0.0810003000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16220
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.267
_diffrn_reflns_theta_min         3.831
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81917
_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    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0047P)^2^+12.2243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3605
_reflns_number_total             3834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj03_lt
_cod_depositor_comments
'Adding full bibliography for 7061279--7061288.cif.'
_cod_database_code               7061280
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N O P'
_reflns_odcompleteness_completeness 94.12
_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 Ternary CH refined with riding coordinates:
 C6(H6), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C25(H25A,H25B), C24(H24A,H24B),
 C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C9(H9), C11(H11), C10(H10), C8(H8), C15(H15), C16(H16)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              33713
_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 3.435
_oxdiff_exptl_absorpt_empirical_full_min 0.525