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_7061281
_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         'C45 H50 Cl O7 P2 Rh, C6 H14'
_chemical_formula_sum            'C51 H64 Cl O7 P2 Rh'
_chemical_formula_weight         989.32
_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                81.1970(10)
_cell_angle_beta                 87.7150(10)
_cell_angle_gamma                72.921(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1330(2)
_cell_length_b                   12.3022(2)
_cell_length_c                   16.7869(3)
_cell_measurement_reflns_used    37023
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      78.7250
_cell_measurement_theta_min      2.6500
_cell_volume                     2366.91(7)
_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      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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -83.00   2.00   0.50    0.22    --  -46.95 104.00-157.00  170
  2  \w      2.00  83.00   0.50    0.22    --   46.95-104.00 101.00  162
  3  \w   -175.00 -85.00   0.50    1.00    -- -102.00-104.00 101.00  180
  4  \w     89.00 178.00   0.50    1.00    --  110.25 104.00-157.00  178
  5  \w     38.00 107.00   0.50    1.00    --  110.25-104.00 101.00  138
  6  \w   -119.00 -74.00   0.50    0.22    --  -46.95-125.00 -90.00   90
  7  \w   -119.00 -74.00   0.50    0.22    --  -46.95-125.00 150.00   90
  8  \w     -5.00  29.00   0.50    0.22    --  -46.95  19.00-150.00   68
  9  \w    -33.00  26.00   0.50    0.22    --  -46.95  37.00  60.00  118
 10  \w     -5.00  29.00   0.50    0.22    --  -46.95  19.00   0.00   68
 11  \w    -26.00  41.00   0.50    0.22    --   46.95 -37.00-180.00  134
 12  \w    -27.00  13.00   0.50    0.22    --   46.95 -19.00-150.00   80
 13  \w     18.00  95.00   0.50    0.22    --   46.95-125.00  60.00  154
 14  \w    -27.00  13.00   0.50    0.22    --   46.95 -19.00  60.00   80
 15  \w   -122.00 -29.00   0.50    1.00    -- -102.00 139.00-103.73  186
 16  \w   -174.00 -88.00   0.50    1.00    -- -102.00 -54.00-172.64  172
 17  \w   -174.00 -88.00   0.50    1.00    -- -102.00 -50.00 142.38  172
 18  \w   -119.00 -29.00   0.50    1.00    -- -102.00 135.00  28.58  180
 19  \w   -126.00 -29.00   0.50    1.00    -- -102.00 144.00 -48.25  194
 20  \w   -119.00 -29.00   0.50    1.00    -- -102.00 135.00-168.44  180
 21  \w   -174.00 -89.00   0.50    1.00    -- -102.00 -45.00-150.00  170
 22  \w   -127.00 -29.00   0.50    1.00    -- -102.00 146.00 121.86  196
 23  \w   -106.00 -29.00   0.50    1.00    -- -102.00 104.00-157.00  154
 24  \w     38.00 111.00   0.50    1.00    --  110.25-125.00  90.00  146
 25  \w     38.00 111.00   0.50    1.00    --  110.25-125.00-150.00  146
 26  \w     38.00 111.00   0.50    1.00    --  110.25-125.00  30.00  146
 27  \w     98.00 178.00   0.50    1.00    --  110.25  30.00 120.00  160
 28  \w     38.00 111.00   0.50    1.00    --  110.25-125.00 150.00  146
 29  \w     88.00 178.00   0.50    1.00    --  110.25  77.00  60.00  180
 30  \w     79.00 178.00   0.50    1.00    --  110.25 125.00-120.00  198
 31  \w     38.00 106.00   0.50    1.00    --  110.25 -94.00 -60.00  136
 32  \w     38.00 111.00   0.50    1.00    --  110.25-125.00 -90.00  146
 33  \w     38.00 111.00   0.50    1.00    --  110.25-125.00  60.00  146
 34  \w     38.00  80.00   0.50    1.00    --  110.25 -61.00   0.00   84
 35  \w     79.00 178.00   0.50    1.00    --  110.25 125.00  30.00  198
 36  \w     38.00 111.00   0.50    1.00    --  110.25-125.00 120.00  146
 37  \w     38.00 111.00   0.50    1.00    --  110.25-125.00-180.00  146
 38  \w     38.00  80.00   0.50    1.00    --  110.25 -61.00  90.00   84
 39  \w     97.00 175.00   0.50    1.00    --  110.25  15.00-180.00  156
 40  \w     98.00 178.00   0.50    1.00    --  110.25  45.00-150.00  160
 41  \w     38.00  80.00   0.50    1.00    --  110.25 -61.00 -60.00   84
 42  \w     38.00 111.00   0.50    1.00    --  110.25-125.00-120.00  146
 43  \w     98.00 178.00   0.50    1.00    --  110.25  30.00   0.00  160
 44  \w     38.00 111.00   0.50    1.00    --  110.25-125.00   0.00  146
 45  \w     98.00 178.00   0.50    1.00    --  110.25  45.00  30.00  160
 46  \w     38.00 111.00   0.50    1.00    --  110.25-125.00 -60.00  146
 47  \w     38.00  80.00   0.50    1.00    --  110.25 -61.00 -30.00   84
 48  \w     -5.00  29.00   0.50    0.22    --  -46.95  19.00-180.00   68
 49  \w     24.00 119.00   0.50    0.22    --   46.95  77.00-180.00  190
 50  \w     32.00 118.00   0.50    0.22    --   46.95  57.00 -90.00  172
 51  \w     32.00 118.00   0.50    0.22    --   46.95  57.00  30.00  172
 52  \w     32.00 118.00   0.50    0.22    --   46.95  57.00 150.00  172
 53  \w     24.00 119.00   0.50    0.22    --   46.95  77.00  60.00  190
 54  \w     24.00 119.00   0.50    0.22    --   46.95  77.00 -90.00  190
 55  \w     24.00 113.00   0.50    0.22    --   46.95  77.00   0.00  178
 56  \w     24.00 119.00   0.50    0.22    --   46.95  77.00 -60.00  190
;
_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      0.0670730000
_diffrn_orient_matrix_UB_12      -0.0207215000
_diffrn_orient_matrix_UB_13      -0.0788163000
_diffrn_orient_matrix_UB_21      0.0752720000
_diffrn_orient_matrix_UB_22      -0.1169644000
_diffrn_orient_matrix_UB_23      0.0421557000
_diffrn_orient_matrix_UB_31      -0.0864858000
_diffrn_orient_matrix_UB_32      -0.0586172000
_diffrn_orient_matrix_UB_33      -0.0252024000
_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  0.0530
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55295
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.128
_diffrn_reflns_theta_min         2.664
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71609
_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    1.388
_exptl_crystal_description       Block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         9288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0558P)^2^+3.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8670
_reflns_number_total             9288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj18_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_database_code               7061281
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N4 O7 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 Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C7(H7A,H7B), C33(H33A,H33B), C36(H36A,H36B), C57(H57A,H57B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
2.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C16(H16), C13(H13), C45(H45), C42(H42), C49(H49), C15(H15),
 C41(H41), C19(H19), C22(H22), C23(H23), C14(H14), C21(H21), C46(H46), C47(H47),
  C40(H40), C20(H20), C39(H39)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C51(H51A,H51B,H51C), C27(H27A,H27B,
 H27C), C53(H53A,H53B,H53C), C28(H28A,H28B,H28C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              8332
_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 2.085
_oxdiff_exptl_absorpt_empirical_full_min 0.602