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_7061283
_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         'C20 H27 P Se'
_chemical_formula_sum            'C20 H27 P Se'
_chemical_formula_weight         377.37
_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             2020-11-06
_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                 91.7860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8601(2)
_cell_length_b                   17.0706(2)
_cell_length_c                   14.00900(10)
_cell_measurement_reflns_used    28272
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.2520
_cell_measurement_theta_min      2.6240
_cell_volume                     3790.97(7)
_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      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.965
_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     34.00 120.00   0.50    0.05    --   47.20  52.00 160.00  172
  2  \w     84.00 110.00   0.50    0.15    --  104.75  77.00-180.00   52
  3  \w    121.00 162.00   0.50    0.15    --  104.75  77.00-180.00   82
  4  \w    133.00 159.00   0.50    0.15    --  104.75  61.00-180.00   52
  5  \w     88.00 116.00   0.50    0.15    --  104.75  61.00-180.00   56
  6  \w     99.00 159.00   0.50    0.15    --  104.75  30.00 -90.00  120
  7  \w     91.00 168.00   0.50    0.15    --  104.75  15.00-120.00  154
  8  \w    115.00 175.00   0.50    0.15    --  104.75  45.00  60.00  120
  9  \w     92.00 176.00   0.50    0.15    --  104.75  45.00  90.00  168
 10  \w     91.00 177.00   0.50    0.15    --  104.75  52.00 160.00  172
 11  \w     80.00 177.00   0.50    0.15    --  104.75 125.00  60.00  194
 12  \w     48.00  80.00   0.50    0.15    --  104.75 -61.00  60.00   64
 13  \w     32.00  64.00   0.50    0.15    --  104.75 -52.00  15.00   64
 14  \w    -24.00  61.00   0.50    0.05    --   47.20 -52.00  15.00  170
 15  \w     42.00  80.00   0.50    0.15    --  104.75 -61.00-120.00   76
 16  \w     18.00  95.00   0.50    0.05    --   47.20-125.00-180.00  154
 17  \w     54.00  80.00   0.50    0.15    --  104.75 -94.00 -90.00   52
 18  \w     45.00  88.00   0.50    0.15    --  104.75 -94.00 -30.00   86
 19  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00 -60.00   64
 20  \w    -55.00  25.00   0.50    0.05    --  -47.20  52.00 160.00  160
 21  \w    -55.00 -29.00   0.50    0.15    -- -102.00  52.00 160.00   52
 22  \w    -72.00 -29.00   0.50    0.15    -- -102.00  61.00 120.00   86
 23  \w    -71.00 -29.00   0.50    0.15    -- -102.00  61.00 -60.00   84
 24  \w    -57.00 -29.00   0.50    0.15    -- -102.00  61.00-180.00   56
 25  \w   -120.00 -33.00   0.50    0.05    --  -47.20 -52.00  15.00  174
 26  \w   -174.00 -88.00   0.50    0.15    -- -102.00 -52.00  15.00  172
 27  \w   -168.00-111.00   0.50    0.15    -- -102.00 -15.00  60.00  114
 28  \w   -174.00-108.00   0.50    0.15    -- -102.00 -45.00 -90.00  132
 29  \w   -175.00 -84.00   0.50    0.15    -- -102.00 -94.00   0.00  182
 30  \w   -120.00 -74.00   0.50    0.05    --  -47.20-125.00  90.00   92
 31  \w   -174.00-147.00   0.50    0.15    -- -102.00-125.00-180.00   54
 32  \w   -119.00 -93.00   0.50    0.15    -- -102.00-125.00-180.00   52
;
_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      0.0860916000
_diffrn_orient_matrix_UB_12      0.0022974000
_diffrn_orient_matrix_UB_13      0.0539165000
_diffrn_orient_matrix_UB_21      -0.0363511000
_diffrn_orient_matrix_UB_22      0.0569764000
_diffrn_orient_matrix_UB_23      0.0734800000
_diffrn_orient_matrix_UB_31      -0.0267237000
_diffrn_orient_matrix_UB_32      -0.0699686000
_diffrn_orient_matrix_UB_33      0.0615636000
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33486
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.430
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86540
_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    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             1573
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.157
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0428P)^2^+3.9755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7273
_reflns_number_total             7673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj06_lt
_cod_depositor_comments
;
Adding full bibliography for 7061279--7061288.cif.

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions. Also removing some strange small boron content
                miguel
;
_cod_original_formula_sum            'C40 H54 B0.25 P2 Se2'
_cod_original_formula_weight         757.39
_cod_original_formula_moiety         '2(C20 H27 P Se)'
_cod_original_formula_units_Z            4
_cod_database_code               7061283
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N O P Se'
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C30(H30), C34(H34), C24(H24), C8(H8), C2(H2), C27(H27), C32(H32),
 C25(H25), C3(H3), C4(H4), C31(H31), C12(H12), C33(H33), C26(H26), C11(H11),
 C10(H10), C9(H9)
2.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C20(H20A,H20B,H20C), C38(H38A,H38B,H38C), C43(H43A,H43B,
 H43C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C18(H18A,H18B,H18C), C41(H41A,
 H41B,H41C), C44(H44A,H44B,H44C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              79510
_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 3.034
_oxdiff_exptl_absorpt_empirical_full_min 0.578