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_7061288
_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         'C53 H70 Cl O5 P2 Rh'
_chemical_formula_sum            'C53 H70 Cl O5 P2 Rh'
_chemical_formula_weight         987.39
_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     iterative
_audit_creation_date             2021-10-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                63.5760(10)
_cell_angle_beta                 86.7820(10)
_cell_angle_gamma                84.9520(10)
_cell_formula_units_Z            2
_cell_length_a                   12.08700(10)
_cell_length_b                   14.5363(2)
_cell_length_c                   15.7989(2)
_cell_measurement_reflns_used    85391
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      78.9260
_cell_measurement_theta_min      3.1150
_cell_volume                     2475.77(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.971
_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     24.00 119.00   0.50    0.05    --   46.95  77.00-120.00  190
  2  \w     24.00 119.00   0.50    0.05    --   46.95  77.00 -60.00  190
  3  \w     24.00 119.00   0.50    0.05    --   46.95  77.00   0.00  190
  4  \w     24.00 119.00   0.50    0.05    --   46.95  77.00  60.00  190
  5  \w     35.00 120.00   0.50    0.05    --   46.95  37.00  60.00  170
  6  \w     35.00 120.00   0.50    0.05    --   46.95  37.00 150.00  170
  7  \w     32.00 118.00   0.50    0.05    --   46.95  57.00 150.00  172
  8  \w     28.00 119.00   0.50    0.05    --   46.95  67.00 177.00  182
  9  \w    -66.00  26.00   0.50    0.05    --  -46.95  67.00 177.00  184
 10  \w    -87.00 -29.00   0.50    0.05    -- -102.00  67.00 177.00  116
 11  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00 150.00   86
 12  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00  30.00   86
 13  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00   0.00   86
 14  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00 -30.00   86
 15  \w    -72.00 -29.00   0.50    0.05    -- -102.00  61.00 -60.00   86
 16  \w     92.00 178.00   0.50    0.05    --  110.25  67.00 177.00  172
 17  \w     94.00 178.00   0.50    0.05    --  110.25  61.00 150.00  168
 18  \w     94.00 178.00   0.50    0.05    --  110.25  61.00 120.00  168
 19  \w     98.00 178.00   0.50    0.05    --  110.25  45.00  90.00  160
 20  \w     98.00 178.00   0.50    0.05    --  110.25  30.00  60.00  160
 21  \w     97.00 175.00   0.50    0.05    --  110.25  15.00 -90.00  156
 22  \w     98.00 178.00   0.50    0.05    --  110.25  30.00-120.00  160
 23  \w     94.00 178.00   0.50    0.05    --  110.25  61.00-150.00  168
 24  \w     79.00 178.00   0.50    0.05    --  110.25 125.00-180.00  198
 25  \w     79.00 178.00   0.50    0.05    --  110.25 125.00 120.00  198
 26  \w     38.00  95.00   0.50    0.05    --  110.25 -67.00  43.00  114
 27  \w    -25.00  66.00   0.50    0.05    --   46.95 -67.00  43.00  182
 28  \w     38.00 133.00   0.50    0.05    --  110.25 -77.00 150.00  190
 29  \w     38.00 117.00   0.50    0.05    --  110.25-133.00 133.67  158
 30  \w     38.00 111.00   0.50    0.05    --  110.25-125.00 150.00  146
 31  \w     38.00 116.00   0.50    0.05    --  110.25-131.00  25.38  156
 32  \w     38.00 111.00   0.50    0.05    --  110.25-125.00  90.00  146
 33  \w     18.00  95.00   0.50    0.05    --   46.95-125.00  60.00  154
 34  \w     38.00 106.00   0.50    0.05    --  110.25 -94.00  90.00  136
 35  \w     38.00 111.00   0.50    0.05    --  110.25-125.00 -60.00  146
 36  \w     38.00 111.00   0.50    0.05    --  110.25-125.00 -90.00  146
 37  \w     38.00 111.00   0.50    0.05    --  110.25-125.00-150.00  146
 38  \w     38.00 106.00   0.50    0.05    --  110.25 -94.00-150.00  136
 39  \w     38.00 106.00   0.50    0.05    --  110.25 -94.00 -90.00  136
 40  \w     38.00 106.00   0.50    0.05    --  110.25 -94.00 -60.00  136
 41  \w     38.00 106.00   0.50    0.05    --  110.25 -94.00  30.00  136
 42  \w     18.00  95.00   0.50    0.05    --   46.95-125.00-120.00  154
 43  \w   -119.00 -24.00   0.50    0.05    --  -46.95 -77.00 -30.00  190
 44  \w   -119.00 -28.00   0.50    0.05    --  -46.95 -67.00  43.00  182
 45  \w   -119.00 -24.00   0.50    0.05    --  -46.95 -77.00-120.00  190
 46  \w   -119.00 -74.00   0.50    0.05    --  -46.95-125.00-180.00   90
 47  \w   -174.00 -89.00   0.50    0.05    -- -102.00 -45.00 -60.00  170
 48  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -77.00 -60.00  192
 49  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -77.00-150.00  192
 50  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -77.00-180.00  192
 51  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -77.00 -90.00  192
 52  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -76.00 -25.63  192
 53  \w   -175.00 -80.00   0.50    0.05    -- -102.00 -78.00  -2.10  190
 54  \w   -175.00 -80.00   0.50    0.05    -- -102.00 -75.00 -41.39  190
 55  \w   -175.00 -80.00   0.50    0.05    -- -102.00 -75.00  19.88  190
 56  \w   -175.00 -80.00   0.50    0.05    -- -102.00 -74.00  37.85  190
 57  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -77.00 150.00  192
 58  \w   -175.00 -81.00   0.50    0.05    -- -102.00 -73.00 132.12  188
 59  \w   -175.00 -79.00   0.50    0.05    -- -102.00 -77.00  90.00  192
 60  \w   -175.00 -82.00   0.50    0.05    -- -102.00 -71.00 118.98  186
 61  \w   -175.00 -81.00   0.50    0.05    -- -102.00 -72.00  72.94  188
 62  \w   -175.00 -83.00   0.50    0.05    -- -102.00 -67.00  43.00  184
 63  \w   -175.00 -80.00   0.50    0.05    -- -102.00 -74.00   8.03  190
 64  \w   -175.00 -83.00   0.50    0.05    -- -102.00 -67.00  53.30  184
 65  \w   -175.00 -83.00   0.50    0.05    -- -102.00 -67.00 155.76  184
 66  \w   -175.00 -84.00   0.50    0.05    -- -102.00 -64.00 -92.68  182
 67  \w   -175.00 -82.00   0.50    0.05    -- -102.00 -71.00-123.54  186
 68  \w   -175.00 -84.00   0.50    0.05    -- -102.00 -65.00-119.17  182
 69  \w   -175.00 -80.00   0.50    0.05    -- -102.00 -74.00-141.67  190
 70  \w   -175.00 -82.00   0.50    0.05    -- -102.00 -69.00-177.11  186
 71  \w   -174.00 -87.00   0.50    0.05    -- -102.00 -56.00 -69.64  174
 72  \w   -174.00 -87.00   0.50    0.05    -- -102.00 -56.00 -18.98  174
 73  \w   -174.00 -86.00   0.50    0.05    -- -102.00 -60.00  94.79  176
 74  \w   -125.00 -29.00   0.50    0.05    -- -102.00 143.00 133.69  192
 75  \w   -120.00 -29.00   0.50    0.05    -- -102.00 136.00 105.23  182
 76  \w   -122.00 -29.00   0.50    0.05    -- -102.00 139.00  -8.71  186
 77  \w   -112.00 -29.00   0.50    0.05    -- -102.00 125.00 -60.00  166
 78  \w   -120.00 -29.00   0.50    0.05    -- -102.00 137.00 -65.14  182
 79  \w   -119.00 -29.00   0.50    0.05    -- -102.00 135.00-177.57  180
 80  \w   -112.00 -29.00   0.50    0.05    -- -102.00 125.00-150.00  166
;
_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      0.0759042000
_diffrn_orient_matrix_UB_12      0.0601460000
_diffrn_orient_matrix_UB_13      0.0294355000
_diffrn_orient_matrix_UB_21      -0.0488936000
_diffrn_orient_matrix_UB_22      0.1020137000
_diffrn_orient_matrix_UB_23      -0.0782783000
_diffrn_orient_matrix_UB_31      -0.0906952000
_diffrn_orient_matrix_UB_32      0.0071378000
_diffrn_orient_matrix_UB_33      0.0697609000
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            101813
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.018
_diffrn_reflns_theta_min         3.124
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.97a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       Block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         10398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.7843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10125
_reflns_number_total             10398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj14_lt_auto
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7061279--7061288.cif.
;
_cod_original_cell_volume        2475.77(5)
_cod_database_code               7061288
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N P2 O3 Rh Cl'
_reflns_odcompleteness_completeness 99.85
_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:
 C45(H45), C51(H51), C16(H16), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C50(H50A,H50B), C27(H27A,H27B), C46(H46A,H46B), C49(H49A,
 H49B), C21(H21A,H21B), C17(H17A,H17B), C55(H55A,H55B), C23(H23A,H23B),
 C52(H52A,H52B), C26(H26A,H26B), C20(H20A,H20B), C24(H24A,H24B), C48(H48A,H48B),
  C25(H25A,H25B), C47(H47A,H47B), C53(H53A,H53B), C54(H54A,H54B), C19(H19A,
 H19B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C43(H43), C42(H42), C5(H5), C11(H11), C13(H13), C40(H40), C12(H12),
 C41(H41), C6(H6), C7(H7), C34(H34), C36(H36), C35(H35)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C58(H58A,H58B,H58C), C60(H60A,H60B,
 H60C)
;
_shelx_res_checksum              75925
_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 1.675
_oxdiff_exptl_absorpt_empirical_full_min 0.718