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_1564647
_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
'C10 H15 Fe I P5, Al C16 F36 O4, 0.5(C6 H4 F2)'
_chemical_formula_sum            'C29 H17 Al F37 Fe I O4 P5'
_chemical_formula_weight         1497.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-23
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.644(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.0024(8)
_cell_length_b                   19.5946(3)
_cell_length_c                   19.9635(6)
_cell_measurement_reflns_used    17399
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      74.6020
_cell_measurement_theta_min      2.8100
_cell_volume                     9602.7(7)
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_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     61.00 132.00   1.00   12.50    --   44.33 178.00-180.00   71
  2  \w    -25.00  68.00   1.00   12.50    --   44.33 -57.00 -90.00   93
  3  \w     36.00  72.00   1.00   50.00    --  104.50 -45.00 -30.00   36
  4  \w     33.00 127.00   1.00   50.00    --  104.50 -77.00 150.00   94
  5  \w     36.00  72.00   1.00   50.00    --  104.50 -45.00 -90.00   36
  6  \w     35.00  93.00   1.00   50.00    --  104.50 -61.00   0.00   58
  7  \w     24.00 107.00   1.00   50.00    --  104.50 -95.00   0.00   83
  8  \w     79.00 174.00   1.00   50.00    --  104.50  61.00 -90.00   95
  9  \w     35.00  93.00   1.00   50.00    --  104.50 -61.00-150.00   58
 10  \w     35.00  93.00   1.00   50.00    --  104.50 -61.00 150.00   58
 11  \w     97.00 176.00   1.00   50.00    --  104.50 125.00-150.00   79
 12  \w     20.00  68.00   1.00   12.50    --   44.33  57.00-120.00   48
 13  \w     20.00 114.00   1.00   12.50    --   44.33  57.00  30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0190032938
_diffrn_orient_matrix_UB_12      -0.0591949991
_diffrn_orient_matrix_UB_13      0.0486681304
_diffrn_orient_matrix_UB_21      -0.0525172418
_diffrn_orient_matrix_UB_22      -0.0268369816
_diffrn_orient_matrix_UB_23      -0.0504853255
_diffrn_orient_matrix_UB_31      0.0098892562
_diffrn_orient_matrix_UB_32      -0.0286843928
_diffrn_orient_matrix_UB_33      -0.0532631687
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39627
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         74.464
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.267
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.163
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         13047
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0602P)^2^+12.3771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11680
_reflns_number_total             13047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr444_cub_mc_abs_gaus
_cod_original_cell_volume        9602.7(6)
_cod_database_code               1564647
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H17AlF37FeIO4P5
_shelx_estimated_absorpt_t_max   0.384
_shelx_estimated_absorpt_t_min   0.131
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.47
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21B-C19 \\sim C21A-C19 \\sim C22B-C19 \\sim C22A-C19 \\sim C20A-C19 \\sim
C20B-C19
 with sigma of 0.02
 P5B-P1B \\sim P1A-P2A
 with sigma of 0.01
 P3A-P2A \\sim P2B-P1B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C25B \\sim C25A \\sim C23: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F36B \\sim F30A \\sim C26B \\sim C24A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
F20B \\sim F21A \\sim C20A \\sim C20B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
P1A \\sim P5B \\sim P4B \\sim P5A \\sim P3B \\sim P4A: within 2.3A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2.3A
C21A \\sim C21B: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.9A
C21B \\sim C21A \\sim C22B \\sim C22A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
4. Others
 Fixed Sof: I1A(0.5) I1B(0.25) P1B(0.5) P4A(0.5) P5A(0.5) P1A(0.5) F24A(0.87)
 F20B(0.87) F23A(0.87) F21B(0.87) F27A(0.87) F26A(0.87) F36A(0.77) F33A(0.77)
 C21A(0.87) C20B(0.87) C26A(0.77) C22A(0.87) C25A(0.77) C28(0.5) C27(0.5)
 C32(0.5) H32(0.5) C31(0.5) H31(0.5) C30(0.5) H30(0.5) C29(0.5) H29(0.5)
 F38(0.5) F37(0.5) I1C(0.25) F23B(0.13) C21B(0.13) F24B(0.13) C20A(0.13)
 F21A(0.13) F20A(0.13) F26B(0.13) C22B(0.13) F27B(0.13) P3B(0.5) P4B(0.5)
 P5B(0.5) P2B(0.5) C24A(0.77) F30A(0.77) C25B(0.23) C26B(0.23) C24B(0.23)
 F30B(0.23) F36B(0.23) F33B(0.23) P3A(0.5) P2A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C31(H31), C30(H30), C29(H29)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              64616
_shelx_hkl_checksum              77052
_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 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.736