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_7061282
_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         'C46 H54 Cl2 O6 P2 Rh2, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H58 Cl6 O6 P2 Rh2'
_chemical_formula_weight         1211.40
_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             2021-11-04
_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                90
_cell_angle_beta                 100.1220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.84410(10)
_cell_length_b                   16.21440(10)
_cell_length_c                   21.0762(2)
_cell_measurement_reflns_used    71127
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      78.9760
_cell_measurement_theta_min      3.0090
_cell_volume                     4993.84(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 0.986
_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     32.00 118.00   0.50    0.10    --   46.95  58.00-110.00  172
  2  \w     24.00 119.00   0.50    0.10    --   46.95  77.00 -60.00  190
  3  \w     35.00 120.00   0.50    0.10    --   46.95  37.00 -90.00  170
  4  \w     35.00 120.00   0.50    0.10    --   46.95  37.00   0.00  170
  5  \w     24.00 119.00   0.50    0.10    --   46.95  77.00  30.00  190
  6  \w     24.00 119.00   0.50    0.10    --   46.95  77.00  90.00  190
  7  \w     24.00 119.00   0.50    0.10    --   46.95  77.00 150.00  190
  8  \w     94.00 178.00   0.50    0.53    --  110.25  61.00 -90.00  168
  9  \w     95.00 178.00   0.50    0.53    --  110.25  58.00-110.00  166
 10  \w     98.00 178.00   0.50    0.53    --  110.25  45.00-180.00  160
 11  \w     98.00 178.00   0.50    0.53    --  110.25  45.00-150.00  160
 12  \w     98.00 178.00   0.50    0.53    --  110.25  45.00 -60.00  160
 13  \w     98.00 178.00   0.50    0.53    --  110.25  45.00 -30.00  160
 14  \w     98.00 178.00   0.50    0.53    --  110.25  45.00 150.00  160
 15  \w     98.00 178.00   0.50    0.53    --  110.25  45.00  60.00  160
 16  \w     97.00 175.00   0.50    0.53    --  110.25  15.00  30.00  156
 17  \w     38.00  74.00   0.50    0.53    --  110.25 -58.00 107.00   72
 18  \w     38.00  80.00   0.50    0.53    --  110.25 -61.00 150.00   84
 19  \w     38.00 133.00   0.50    0.53    --  110.25 -77.00 150.00  190
 20  \w     38.00  80.00   0.50    0.53    --  110.25 -61.00  60.00   84
 21  \w     38.00  80.00   0.50    0.53    --  110.25 -61.00  30.00   84
 22  \w     38.00  80.00   0.50    0.53    --  110.25 -61.00   0.00   84
 23  \w     38.00  80.00   0.50    0.53    --  110.25 -61.00 -60.00   84
 24  \w     38.00  80.00   0.50    0.53    --  110.25 -61.00-180.00   84
 25  \w     38.00 106.00   0.50    0.53    --  110.25 -94.00 -90.00  136
 26  \w     38.00 106.00   0.50    0.53    --  110.25 -94.00-120.00  136
 27  \w     38.00 111.00   0.50    0.53    --  110.25-125.00-180.00  146
 28  \w     38.00 111.00   0.50    0.53    --  110.25-125.00  30.00  146
 29  \w     38.00 111.00   0.50    0.53    --  110.25-125.00  90.00  146
 30  \w     38.00 111.00   0.50    0.53    --  110.25-125.00 120.00  146
 31  \w    -27.00  13.00   0.50    0.10    --   46.95 -19.00 150.00   80
 32  \w     79.00 178.00   0.50    0.53    --  110.25 125.00  90.00  198
 33  \w    -24.00  62.00   0.50    0.10    --   46.95 -58.00 107.00  172
 34  \w   -119.00 -74.00   0.50    0.10    --  -46.95-125.00 -90.00   90
 35  \w   -175.00 -84.00   0.50    0.53    -- -102.00 -94.00-180.00  182
 36  \w   -175.00-136.00   0.50    0.53    -- -102.00 -77.00-150.00   78
 37  \w   -175.00 -79.00   0.50    0.53    -- -102.00 -77.00-120.00  192
 38  \w   -175.00 -79.00   0.50    0.53    -- -102.00 -77.00 -90.00  192
 39  \w   -175.00 -79.00   0.50    0.53    -- -102.00 -77.00  30.00  192
 40  \w   -175.00 -79.00   0.50    0.53    -- -102.00 -77.00  60.00  192
 41  \w   -174.00 -87.00   0.50    0.53    -- -102.00 -58.00 107.00  174
 42  \w   -175.00 -79.00   0.50    0.53    -- -102.00 -77.00  90.00  192
 43  \w   -175.00 -79.00   0.50    0.53    -- -102.00 -77.00 150.00  192
 44  \w   -118.00 -32.00   0.50    0.10    --  -46.95 -58.00 107.00  172
 45  \w     -5.00  29.00   0.50    0.10    --  -46.95  19.00  30.00   68
 46  \w    -62.00  26.00   0.50    0.10    --  -46.95  58.00-110.00  176
 47  \w    -66.00 -29.00   0.50    0.53    -- -102.00  58.00-110.00   74
 48  \w    -72.00 -29.00   0.50    0.53    -- -102.00  61.00 -60.00   86
 49  \w    -72.00 -29.00   0.50    0.53    -- -102.00  61.00  30.00   86
;
_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      -0.0735539000
_diffrn_orient_matrix_UB_12      0.0650779000
_diffrn_orient_matrix_UB_13      0.0059992000
_diffrn_orient_matrix_UB_21      0.0281433000
_diffrn_orient_matrix_UB_22      -0.0018037000
_diffrn_orient_matrix_UB_23      0.0739287000
_diffrn_orient_matrix_UB_31      0.0699891000
_diffrn_orient_matrix_UB_32      0.0692336000
_diffrn_orient_matrix_UB_33      -0.0038298000
_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  0.0587
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.183
_diffrn_reflns_theta_min         3.024
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62090
_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    1.611
_exptl_crystal_description       Blade
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         10654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0479P)^2^+8.2355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9909
_reflns_number_total             10654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj15_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               7061282
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N O4 Rh Cl P2'
_reflns_odcompleteness_completeness 100.00
_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:
 C5(H5), C9(H9), C34(H34), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C28(H28A,H28B), C27(H27A,H27B), C26(H26A,H26B),
 C6(H6A,H6B), C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B), C53(H53A,H53B),
 C51(H51A,H51B), C52(H52A,H52B), C59(H59A,H59B), C56(H56A,H56B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C39(H39), C36(H36), C14(H14), C13(H13), C12(H12), C37(H37),
 C38(H38), C45(H45), C18(H18), C20(H20), C43(H43), C44(H44), C19(H19)
2.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              44111
_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 2.043
_oxdiff_exptl_absorpt_empirical_full_min 0.565