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_7061284
_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
'C41 H46 Cl O P2 Rh, C H2 Cl2, C0.59 H1.18 Cl1.17, C0.41 H0.82 Cl0.83'
_chemical_formula_sum            'C43 H50 Cl5 O P2 Rh'
_chemical_formula_weight         924.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2022-01-18 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            8
_cell_length_a                   17.93190(10)
_cell_length_b                   17.95520(10)
_cell_length_c                   26.01420(10)
_cell_measurement_reflns_used    68804
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      78.8450
_cell_measurement_theta_min      2.9240
_cell_volume                     8375.81(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 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 0.989
_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     33.00 118.00   0.50    0.06    --   46.95  52.00 129.00  170
  2  \w     98.00 178.00   0.50    0.20    --  110.25  45.00 120.00  160
  3  \w     98.00 178.00   0.50    0.20    --  110.25  30.00  90.00  160
  4  \w     98.00 178.00   0.50    0.20    --  110.25  45.00  30.00  160
  5  \w     98.00 178.00   0.50    0.20    --  110.25  30.00 -30.00  160
  6  \w     98.00 178.00   0.50    0.20    --  110.25  30.00-120.00  160
  7  \w     97.00 175.00   0.50    0.20    --  110.25  15.00-180.00  156
  8  \w     32.00 118.00   0.50    0.06    --   46.95  57.00-120.00  172
  9  \w     88.00 178.00   0.50    0.20    --  110.25 107.00  -2.00  180
 10  \w     38.00  80.00   0.50    0.20    --  110.25 -61.00 -60.00   84
 11  \w     38.00  80.00   0.50    0.20    --  110.25 -61.00 -90.00   84
 12  \w     38.00  80.00   0.50    0.20    --  110.25 -61.00-120.00   84
 13  \w     38.00 133.00   0.50    0.20    --  110.25 -77.00-120.00  190
 14  \w     38.00  64.00   0.50    0.20    --  110.25 -52.00 -16.00   52
 15  \w    -27.00  13.00   0.50    0.06    --   46.95 -19.00 -30.00   80
 16  \w     38.00  80.00   0.50    0.20    --  110.25 -61.00 120.00   84
 17  \w     38.00 106.00   0.50    0.20    --  110.25 -94.00 120.00  136
 18  \w     38.00 111.00   0.50    0.20    --  110.25-125.00  90.00  146
 19  \w     38.00 111.00   0.50    0.20    --  110.25-125.00-120.00  146
 20  \w     18.00  95.00   0.50    0.06    --   46.95-125.00-150.00  154
 21  \w     -5.00  29.00   0.50    0.06    --  -46.95  19.00 -60.00   68
 22  \w     -5.00  29.00   0.50    0.06    --  -46.95  19.00-120.00   68
 23  \w     -5.00  29.00   0.50    0.06    --  -46.95  19.00-180.00   68
 24  \w     -5.00  29.00   0.50    0.06    --  -46.95  19.00 -90.00   68
 25  \w    -56.00 -29.00   0.50    0.20    -- -102.00  52.00 129.00   54
 26  \w   -112.00 -87.00   0.50    0.20    -- -102.00 125.00 -30.00   50
 27  \w   -118.00 -33.00   0.50    0.06    --  -46.95 -52.00 -16.00  170
 28  \w   -175.00 -79.00   0.50    0.20    -- -102.00 -77.00 -60.00  192
 29  \w   -174.00 -88.00   0.50    0.20    -- -102.00 -52.00 -16.00  172
;
_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      -0.0615605000
_diffrn_orient_matrix_UB_12      0.0298518000
_diffrn_orient_matrix_UB_13      0.0358379000
_diffrn_orient_matrix_UB_21      -0.0330994000
_diffrn_orient_matrix_UB_22      0.0451118000
_diffrn_orient_matrix_UB_23      -0.0449022000
_diffrn_orient_matrix_UB_31      -0.0499723000
_diffrn_orient_matrix_UB_32      -0.0665860000
_diffrn_orient_matrix_UB_33      -0.0143737000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            86764
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.147
_diffrn_reflns_theta_min         3.398
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.208
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60531
_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    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+5.9856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8609
_reflns_number_total             8963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05769c2.cif
_cod_data_source_block           cm_uj13_lt_auto
_cod_depositor_comments
'Adding full bibliography for 7061279--7061288.cif.'
_cod_database_code               7061284
_shelxl_version_number           2013-3
_diffrn_oxdiff_digest_frames
;
01b5f7dd97127c66057145813de364c03700064ac8a
;
_diffrn_oxdiff_digest_hkl
;
0197b0faa148b244c30c09f488fc63b3f47d8b
;
_reflns_odcompleteness_completeness 99.90
_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, All C(H,H,H,H) groups
2. Others
 Sof(H9BC)=Sof(H9BD)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(Cl4B)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(Cl4A)=FVAR(1)
 Sof(Cl5B)=1-FVAR(2)
 Sof(Cl5A)=FVAR(2)
 Sof(Cl2B)=1-FVAR(3)
 Sof(Cl2A)=FVAR(3)
 Sof(Cl3B)=1-FVAR(4)
 Sof(Cl3A)=FVAR(4)
3.a Ternary CH refined with riding coordinates:
 C25(H25), C33(H33), C37(H37), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C40(H40A,H40B), C26(H26A,H26B), C28(H28A,H28B), C38(H38A,
 H38B), C32(H32A,H32B), C30(H30A,H30B), C39(H39A,H39B), C27(H27A,H27B),
 C36(H36A,H36B), C31(H31A,H31B), C35(H35A,H35B), C9(H9AA,H9AB), C9(H9BC,H9BD),
 C6A(H6AA,H6AB), C6B(H6BA,H6BB)
3.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C17(H17), C46(H46), C48(H48), C15(H15), C16(H16),
 C24(H24), C51(H51), C23(H23), C42(H42), C45(H45), C21(H21), C50(H50), C22(H22),
  C49(H49), C44(H44), C43(H43)
;
_shelx_res_checksum              96146
_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 1.530
_oxdiff_exptl_absorpt_empirical_full_min 0.719