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_7061285
_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         'C26 H35 O2 P Se'
_chemical_formula_sum            'C26 H35 O2 P Se'
_chemical_formula_weight         489.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.57166(18)
_cell_length_b                   14.50525(17)
_cell_length_c                   9.46339(10)
_cell_measurement_reflns_used    19897
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      76.1580
_cell_measurement_theta_min      3.9230
_cell_volume                     2412.04(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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 -30.00   64
  2  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00   0.00   64
  3  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00 -60.00   64
  4  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00-120.00   64
  5  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00-150.00   64
  6  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00 -90.00   64
  7  \w      3.00  84.00   0.50    0.05    --   47.20-106.00  82.00  162
  8  \w     -4.00  28.00   0.50    0.05    --  -47.20  19.00  90.00   64
  9  \w     25.00 120.00   0.50    0.05    --   47.20  77.00 120.00  190
 10  \w     92.00 178.00   0.50    0.05    --  104.75  30.00  30.00  172
 11  \w     91.00 116.00   0.50    0.05    --  104.75  15.00 -90.00   50
 12  \w     82.00 178.00   0.50    0.05    --  104.75  76.00 -65.00  192
 13  \w     91.00 176.00   0.50    0.05    --  104.75  15.00-180.00  170
 14  \w     32.00  60.00   0.50    0.05    --  104.75 -50.00 -51.00   56
 15  \w     32.00  80.00   0.50    0.05    --  104.75 -61.00-120.00   96
 16  \w     32.00  80.00   0.50    0.05    --  104.75 -61.00  60.00   96
 17  \w     32.00 128.00   0.50    0.05    --  104.75 -77.00 120.00  192
 18  \w     32.00 106.00   0.50    0.05    --  104.75 -94.00  90.00  148
 19  \w     32.00 106.00   0.50    0.05    --  104.75 -94.00 120.00  148
 20  \w     32.00 107.00   0.50    0.05    --  104.75-106.00  82.00  150
 21  \w     32.00 120.00   0.50    0.05    --   47.20  57.00-150.00  176
 22  \w     25.00 120.00   0.50    0.05    --   47.20  77.00  30.00  190
 23  \w     25.00 120.00   0.50    0.05    --   47.20  77.00 -90.00  190
 24  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00  30.00   86
 25  \w   -107.00 -29.00   0.50    0.05    -- -102.00 106.00-178.00  156
;
_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      0.0490931000
_diffrn_orient_matrix_UB_12      -0.0681921000
_diffrn_orient_matrix_UB_13      0.0852873000
_diffrn_orient_matrix_UB_21      0.0196481000
_diffrn_orient_matrix_UB_22      0.0771253000
_diffrn_orient_matrix_UB_23      0.1058926000
_diffrn_orient_matrix_UB_31      -0.0699380000
_diffrn_orient_matrix_UB_32      -0.0260869000
_diffrn_orient_matrix_UB_33      0.0895159000
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21630
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.266
_diffrn_reflns_theta_min         3.952
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60517
_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    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.364
_exptl_crystal_size_min          0.284
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1912 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0407P)^2^+0.6654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.837
_reflns_number_gt                4555
_reflns_number_total             4625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj08_lt
_cod_depositor_comments
;
Adding full bibliography for 7061279--7061288.cif.

2025-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         195.79
_cod_original_formula_moiety         'C10.4 H14 O0.8 P0.4 Se0.4'
_cod_original_formula_units_Z            10
_cod_original_formula_sum        'C10.40 H14 O0.80 P0.40 Se0.40'
_cod_database_code               7061285
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N O P Se'
_reflns_odcompleteness_completeness 99.93
_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:
 C15(H15), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C25(H25A,H25B), C17(H17A,H17B), C18(H18A,H18B), C23(H23A,
 H23B), C19(H19A,H19B), C20(H20A,H20B), C26(H26A,H26B), C21(H21A,H21B),
 C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C3(H3), C5(H5), C14(H14), C13(H13), C12(H12), C4(H4)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              30404
_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 4.670
_oxdiff_exptl_absorpt_empirical_full_min 0.384