Substituted aromatic pentaphosphole ligands ‒ a journey across the p-block
Riesinger, Christoph; Balázs, Gábor; Seidl, Michael; Scheer, Manfred; Chemical Science  (2021) –; doi:10.1039/D1SC04296C

data_1564638
_publ_section_title
;
 Substituted aromatic pentaphosphole ligands -- a journey across the
 p-block
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04296C
_journal_year                    2021
_chemical_formula_moiety
'C20 H30 B Br2 Fe2 P10, Al C16 F36 O4, 0.6[C6H14]'
_chemical_formula_sum            'C39.6 H38.4 Al B Br2 F36 Fe2 O4 P10'
_chemical_formula_weight         1881.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-05
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.870(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.0184(7)
_cell_length_b                   9.73790(10)
_cell_length_c                   18.3964(4)
_cell_measurement_reflns_used    13417
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.7380
_cell_measurement_theta_min      4.3000
_cell_volume                     6450.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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    -84.00 -23.00   1.00   15.00    --  -40.53 122.00 -46.00   61
  2  \w    -40.00  27.00   1.00   15.00    --   40.53 -19.00  30.00   67
  3  \w    -41.00  27.00   1.00   15.00    --   40.53 -19.00 -30.00   68
  4  \w     34.00  71.00   1.00   50.00    --  104.28 -61.00 120.00   37
  5  \w     89.00 171.00   1.00   50.00    --  104.28 111.00  60.00   82
  6  \w     19.00  72.00   1.00   50.00    --  104.28 -90.00-107.10   53
  7  \w     30.00  57.00   1.00   50.00    --  104.28 -61.00  60.00   27
  8  \w     81.00 120.00   1.00   50.00    --  104.28 -90.00-107.10   39
  9  \w     77.00 175.00   1.00   50.00    --  104.28  45.00-150.00   98
 10  \w     21.00 142.00   1.00   50.00    --  104.28 -91.00   1.66  121
 11  \w    -98.00 -18.00   1.00   15.00    --  -41.53 125.00-180.00   80
 12  \w    -39.00  27.00   1.00   15.00    --   41.53 -19.00  90.00   66
 13  \w      5.00  48.00   1.00   15.00    --   41.53 -57.00 120.00   43
 14  \w     79.00 171.00   1.00   50.00    --  104.28 111.00  30.00   92
 15  \w     71.00 105.00   1.00   50.00    --  104.28  77.00 120.00   34
 16  \w    111.00 143.00   1.00   50.00    --  104.28  77.00 120.00   32
 17  \w     21.00  72.00   1.00   50.00    --  104.28 -95.00 -30.00   51
 18  \w    100.00 173.00   1.00   50.00    --  104.28 111.00 150.00   73
 19  \w     89.00 176.00   1.00   50.00    --  104.28  45.00   0.00   87
 20  \w     70.00 124.00   1.00   50.00    --  104.28 -91.00 143.38   54
 21  \w     25.00  51.00   1.00   50.00    --  104.28 -91.00 143.38   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0014287702
_diffrn_orient_matrix_UB_12      0.1557723336
_diffrn_orient_matrix_UB_13      0.0156673275
_diffrn_orient_matrix_UB_21      -0.0425174030
_diffrn_orient_matrix_UB_22      0.0081088508
_diffrn_orient_matrix_UB_23      -0.0487590236
_diffrn_orient_matrix_UB_31      -0.0046290415
_diffrn_orient_matrix_UB_32      -0.0262311028
_diffrn_orient_matrix_UB_33      0.0776865501
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23789
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.039
_diffrn_reflns_theta_min         4.346
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.892
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_description       prism
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.386(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         12143
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0701P)^2^+10.3961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                11912
_reflns_number_total             12143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr378_cua_mc_abs
_cod_original_formula_sum        'C39.60 H38.40 Al B Br2 F36 Fe2 O4 P10'
_cod_database_code               1564638
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AlBBr2C39.6F36Fe2H38.4O4P10
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.142
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.614(5)
 0.386(5)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 F19-C30A \\sim F21A-C30A \\sim F20A-C30A \\sim F21B-C30B \\sim F19-C30B \\sim
F20B-C30B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O3 \\sim C29 \\sim C31B \\sim F22B \\sim F23B \\sim F24 \\sim C30B \\sim F19
\\sim F20B \\sim F21B \\sim C32B \\sim F26B \\sim F27B: within 1.9A with sigma
of 0.01 and sigma for terminal atoms of 0.01 within 1.9A
5. Others
 Fixed Sof: F20A(0.68) F27A(0.68) F23A(0.68) F22A(0.68) F26A(0.68) F21A(0.68)
 C30A(0.68) C32A(0.68) C31A(0.68) C31B(0.32) F22B(0.32) F23B(0.32) C30B(0.32)
 F20B(0.32) F21B(0.32) C32B(0.32) F26B(0.32) F27B(0.32)
6.a Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C7(H7A,H7B,
 H7C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   1.4
_smtbx_masks_void_truncation_radius 1.4
_shelx_res_checksum              61605
_shelx_hkl_checksum              94691
_shelx_fab_checksum              76558
_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 1.809
_oxdiff_exptl_absorpt_empirical_full_min 0.566