In Crystallo Lattice Adaptivity Triggered by Solid-Gas Reactions of Cationic Group 7 Pincer Complexes
Goodall, Joe C.; Sajjad, Muhammad Arif; Thompson, Emily A.; Page, Samuel J.; Kerrigan, Adam M.; Jenkins, Huw T.; Lynam, Jason Martin; Macgregor, Stuart Alan; Weller, Andrew S.; Chemical Communications  (2023) –; doi:10.1039/D3CC03201A

data_7132005
_publ_section_title
;
 In Crystallo Lattice Adaptivity Triggered by Solid-Gas Reactions of
 Cationic Group 7 Pincer Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03201A
_journal_year                    2023
_chemical_formula_moiety         'C24 H39 N O5 P2 Re, C32 H12 B F24'
_chemical_formula_sum            'C56 H51 B F24 N O5 P2 Re'
_chemical_formula_weight         1532.92
_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     dual
_audit_creation_date             2023-06-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-06-22 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                97.370(2)
_cell_angle_beta                 94.209(3)
_cell_angle_gamma                96.468(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9529(4)
_cell_length_b                   14.1717(3)
_cell_length_c                   16.8449(5)
_cell_measurement_reflns_used    17160
_cell_measurement_temperature    109.95(10)
_cell_measurement_theta_max      76.8070
_cell_measurement_theta_min      3.8350
_cell_volume                     3034.93(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109.95(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.950
_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   -122.00 -32.00   0.50    9.61    --  -48.95 -61.00  71.00  180
  2  \w    -61.00  16.00   0.50    9.61    --  -48.95  61.00-150.00  154
  3  \w     50.00  77.00   0.50    9.61    --   48.95  61.00-150.00   54
  4  \w    -23.00  61.00   0.50    9.61    --   48.95 -61.00  71.00  168
  5  \w     38.00 100.00   0.50   38.45    --  107.75 -61.00  71.00  124
  6  \w     92.00 159.00   0.50   38.45    --  107.75  61.00-150.00  134
  7  \w   -114.00 -73.00   0.50    9.61    --  -48.95-125.00-150.00   82
  8  \w    -82.00 -15.00   0.50    9.61    --  -48.95 125.00-120.00  134
  9  \w   -119.00 -73.00   0.50    9.61    --  -48.95-125.00   0.00   92
 10  \w     39.00  78.00   0.50    9.61    --   48.95-125.00 -60.00   78
 11  \w     -7.00  53.00   0.50    9.61    --   48.95 -57.00-180.00  120
 12  \w     46.00  96.00   0.50   38.45    --  107.75-125.00  30.00  100
 13  \w     69.00 101.00   0.50   38.45    --  107.75 -99.00-120.00   64
 14  \w    104.00 151.00   0.50   38.45    --  107.75 125.00 150.00   94
 15  \w     39.00 112.00   0.50   38.45    --  107.75-125.00 120.00  146
 16  \w     95.00 174.00   0.50   38.45    --  107.75  57.00-180.00  158
 17  \w     37.00 106.00   0.50   38.45    --  107.75 -99.00-150.00  138
 18  \w     35.00 121.00   0.50   38.45    --  107.75 -19.00-180.00  172
 19  \w     55.00 106.00   0.50   38.45    --  107.75-125.00  90.00  102
 20  \w     96.00 161.00   0.50   38.45    --  107.75  19.00-180.00  130
 21  \w     58.00 104.00   0.50   38.45    --  107.75 -99.00-180.00   92
 22  \w     37.00 110.00   0.50   38.45    --  107.75 -37.00  60.00  146
 23  \w     53.00 119.00   0.50   38.45    --  107.75 -37.00-180.00  132
 24  \w     61.00 104.00   0.50   38.45    --  107.75 -99.00 -30.00   86
 25  \w    104.00 143.00   0.50   38.45    --  107.75 125.00-150.00   78
 26  \w     76.00 105.00   0.50   38.45    --  107.75 -99.00  30.00   58
 27  \w     95.00 157.00   0.50   38.45    --  107.75 125.00  90.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0317227000
_diffrn_orient_matrix_UB_12      0.0980684000
_diffrn_orient_matrix_UB_13      0.0519766000
_diffrn_orient_matrix_UB_21      -0.0914810000
_diffrn_orient_matrix_UB_22      0.0402492000
_diffrn_orient_matrix_UB_23      -0.0424476000
_diffrn_orient_matrix_UB_31      -0.0711820000
_diffrn_orient_matrix_UB_32      -0.0310360000
_diffrn_orient_matrix_UB_33      0.0637871000
_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  0.0889
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32934
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.598
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.540
_refine_diff_density_min         -2.030
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0855P)^2^+0.0183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10499
_reflns_number_total             12265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03201a2.cif
_cod_data_source_block           asw23009
_cod_database_code               7132005
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H51 B1 F24 Re1 P2 O4 N1'
_chemical_oxdiff_usercomment     'JG098 SCSC'
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.608
_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.a Aromatic/amide H refined with riding coordinates:
 C54(H54), C38(H38), C52(H52), C30(H30), C46(H46), C28(H28), C26(H26),
 C44(H44), C15(H15), C50(H50), C34(H34), C36(H36), C13(H13), C42(H42), C14(H14)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C9(H9A,H9B,
 H9C), C24(H24A,H24B,H24C), C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C5(H5A,H5B,
 H5C)
;
_shelx_res_checksum              16841
_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 2.268
_oxdiff_exptl_absorpt_empirical_full_min 0.523