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_7132000
_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         'C23 H39 N O4 P2 Re, C32 H12 B F24'
_chemical_formula_sum            'C55 H51 B F24 N O4 P2 Re'
_chemical_formula_weight         1504.91
_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                106.7050(10)
_cell_angle_beta                 93.6650(10)
_cell_angle_gamma                98.2320(10)
_cell_formula_units_Z            2
_cell_length_a                   12.87470(10)
_cell_length_b                   14.51620(10)
_cell_length_c                   17.7612(2)
_cell_measurement_reflns_used    29069
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      76.6520
_cell_measurement_theta_min      3.4770
_cell_volume                     3127.18(5)
_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      air
_diffrn_ambient_temperature      298.0(2)
_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 0.965
_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    -74.00  -3.00   0.50    1.00    --  -48.95 112.00  63.00  142
  2  \w     32.00  57.00   0.50    1.00    --   48.95-112.00 -29.00   50
  3  \w    115.00 145.00   0.50    3.05    --  107.75 112.00  63.00   60
  4  \w     51.00 108.00   0.50    3.05    --  107.75-112.00 -29.00  114
  5  \w    -61.00  18.00   0.50    1.00    --  -48.95  37.00 120.00  158
  6  \w   -119.00 -94.00   0.50    1.00    --  -48.95-125.00 150.00   50
  7  \w   -118.00 -91.00   0.50    1.00    --  -48.95-125.00  60.00   54
  8  \w   -122.00 -26.00   0.50    1.00    --  -48.95 -77.00 -30.00  192
  9  \w    -51.00  23.00   0.50    1.00    --  -48.95  37.00  30.00  148
 10  \w   -116.00 -77.00   0.50    1.00    --  -48.95-125.00  30.00   78
 11  \w      7.00  77.00   0.50    1.00    --   48.95 -99.00 -30.00  140
 12  \w     34.00  72.00   0.50    1.00    --   48.95-125.00 -60.00   76
 13  \w     35.00 100.00   0.50    3.05    --  107.75 -37.00 -90.00  130
 14  \w     62.00 106.00   0.50    3.05    --  107.75 -99.00  30.00   88
 15  \w     38.00 121.00   0.50    3.05    --  107.75 -19.00  30.00  166
 16  \w     95.00 159.00   0.50    3.05    --  107.75  37.00  30.00  128
 17  \w     79.00 105.00   0.50    3.05    --  107.75 -99.00 -30.00   52
 18  \w     37.00 106.00   0.50    3.05    --  107.75 -99.00-120.00  138
 19  \w    124.00 166.00   0.50    3.05    --  107.75 125.00 -90.00   84
 20  \w     40.00 117.00   0.50    3.05    --  107.75 -37.00 150.00  154
 21  \w     37.00  87.00   0.50    3.05    --  107.75 -99.00  60.00  100
 22  \w     65.00 106.00   0.50    3.05    --  107.75 -99.00  90.00   82
 23  \w     95.00 165.00   0.50    3.05    --  107.75  37.00 -90.00  140
 24  \w     69.00 111.00   0.50    3.05    --  107.75-125.00-120.00   84
 25  \w     42.00  88.00   0.50    3.05    --  107.75-125.00   0.00   92
 26  \w     58.00  84.00   0.50    3.05    --  107.75 -99.00   0.00   52
 27  \w     98.00 147.00   0.50    3.05    --  107.75 125.00-180.00   98
 28  \w     43.00 120.00   0.50    3.05    --  107.75 -37.00  30.00  154
 29  \w     38.00 107.00   0.50    3.05    --  107.75-125.00-150.00  138
 30  \w     96.00 177.00   0.50    3.05    --  107.75  37.00   0.00  162
;
_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      -0.0091661000
_diffrn_orient_matrix_UB_12      -0.0019698000
_diffrn_orient_matrix_UB_13      0.0856025000
_diffrn_orient_matrix_UB_21      -0.0034188000
_diffrn_orient_matrix_UB_22      0.1102247000
_diffrn_orient_matrix_UB_23      0.0259745000
_diffrn_orient_matrix_UB_31      -0.1212592000
_diffrn_orient_matrix_UB_32      -0.0220223000
_diffrn_orient_matrix_UB_33      -0.0173366000
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37887
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.980
_diffrn_reflns_theta_min         3.489
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87814
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         12765
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.4681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11736
_reflns_number_total             12765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03201a2.cif
_cod_data_source_block           asw23023
_cod_database_code               7132000
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Re1 B1 F24 C55 H51 P2 N1 O4'
_chemical_oxdiff_usercomment     JG091-RT
_shelx_estimated_absorpt_t_max   0.654
_shelx_estimated_absorpt_t_min   0.420
_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
 C31-F6 \\sim C31-F5 \\sim C31-F4A \\sim C31-F5A \\sim C31-F6A \\sim C31-F4
 with sigma of 0.02
 C55-F22 \\sim C55-F24 \\sim C55-F23A \\sim C55-F22A \\sim C55-F24A \\sim
C55-F23
 with sigma of 0.02
 C46-F15 \\sim C46-F14 \\sim C46-F15A \\sim C46-F15A \\sim C46-F15A \\sim
C46-F13
 with sigma of 0.02
 C30-F3 \\sim C30-F2 \\sim C30-F1 \\sim C30-F3A \\sim C30-F2A \\sim C30-F1A
 with sigma of 0.02
 C47-F18 \\sim C47-F16A \\sim C47-F17A \\sim C47-F18A \\sim C47-F17 \\sim
C47-F16
 with sigma of 0.02
 C39-F10 \\sim C39-F12 \\sim C39-F11 \\sim C39-F12A \\sim C39-F10A \\sim
C39-F12A
 with sigma of 0.02
 C38-F9 \\sim C38-F8 \\sim C38-F8A \\sim C38-F9A \\sim C38-F7A \\sim C38-F7
 with sigma of 0.02
 C54-F19 \\sim C54-F21 \\sim C54-F20 \\sim C54-F20A \\sim C54-F19A \\sim
C54-F21A
 with sigma of 0.02
 F6-F5 \\sim F6-F4 \\sim F5-F4 \\sim F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.04
 F19-F20 \\sim F21-F20 \\sim F20A-F19A \\sim F20A-F21A
 with sigma of 0.04
 F9-F8 \\sim F9-F7 \\sim F8-F7 \\sim F8A-F9A \\sim F8A-F7A \\sim F9A-F7A
 with sigma of 0.04
 F18-F17 \\sim F18-F16 \\sim F16A-F17A \\sim F16A-F18A \\sim F17A-F18A \\sim
F17-F16
 with sigma of 0.04
 F10-F12 \\sim F10-F11 \\sim F12-F11 \\sim F12A-F10A \\sim F12A-F11A \\sim
F10A-F11A
 with sigma of 0.04
 F3-F2 \\sim F3-F1 \\sim F2-F1 \\sim F3A-F2A \\sim F3A-F1A \\sim F2A-F1A
 with sigma of 0.04
 F15-F14 \\sim F15-F13 \\sim F14-F13 \\sim F15A-F14A \\sim F15A-F13A \\sim
F14A-F13A
 with sigma of 0.04
 F22-F24 \\sim F22-F23 \\sim F24-F23 \\sim F23A-F22A \\sim F23A-F24A \\sim
F22A-F24A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F10 \\sim F12 \\sim F11: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
F16 \\sim F18 \\sim F17: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
F21 \\sim F19 \\sim F20: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 F11, F12, F10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F18, F16, F17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F20A)=Sof(F19A)=Sof(F21A)=1-FVAR(1)
 Sof(F19)=Sof(F21)=Sof(F20)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F6)=Sof(F5)=FVAR(2)
 Sof(F8A)=Sof(F9A)=Sof(F7A)=1-FVAR(3)
 Sof(F7)=Sof(F9)=Sof(F8)=FVAR(3)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(4)
 Sof(F17)=Sof(F16)=Sof(F18)=FVAR(4)
 Sof(F12A)=Sof(F10A)=Sof(F11A)=1-FVAR(5)
 Sof(F12)=Sof(F10)=Sof(F11)=FVAR(5)
 Sof(F3A)=Sof(F2A)=Sof(F1A)=1-FVAR(6)
 Sof(F2)=Sof(F1)=Sof(F3)=FVAR(6)
 Sof(F15A)=Sof(F14A)=Sof(F13A)=1-FVAR(7)
 Sof(F15)=Sof(F13)=Sof(F14)=FVAR(7)
 Sof(F23A)=Sof(F22A)=Sof(F24A)=1-FVAR(8)
 Sof(F23)=Sof(F24)=Sof(F22)=FVAR(8)
6.a Aromatic/amide H refined with riding coordinates:
 C33(H33), C41(H41), C53(H53), C45(H45), C27(H27), C51(H51), C49(H49),
 C29(H29), C25(H25), C35(H35), C43(H43), C37(H37), C14(H14), C13(H13), C12(H12)
6.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              16479
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.820