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_7132003
_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             2023-06-15
_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                107.7110(10)
_cell_angle_beta                 94.0020(10)
_cell_angle_gamma                98.7510(10)
_cell_formula_units_Z            2
_cell_length_a                   12.74810(10)
_cell_length_b                   14.4679(2)
_cell_length_c                   17.4995(2)
_cell_measurement_reflns_used    29016
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      76.5610
_cell_measurement_theta_min      4.1040
_cell_volume                     3015.63(6)
_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      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_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   -118.00 -93.00   0.50    0.40    --  -50.29-133.00 138.00   50
  2  \w   -116.00 -66.00   0.50    0.40    --  -50.29-136.00 -39.00  100
  3  \w    -81.00 -56.00   0.50    0.40    --  -50.29 136.00  24.00   50
  4  \w    -91.00 -66.00   0.50    0.40    --  -50.29 133.00-153.00   50
  5  \w     49.00  96.00   0.50    0.40    --   50.29-133.00 138.00   94
  6  \w     42.00 102.00   0.50    0.40    --   50.29-136.00 -39.00  120
  7  \w     48.00 117.00   0.50    1.50    --  105.75-133.00 138.00  138
  8  \w     49.00 116.00   0.50    1.50    --  105.75-136.00 -39.00  134
  9  \w    109.00 134.00   0.50    1.50    --  105.75 136.00  24.00   50
 10  \w    133.00 158.00   0.50    1.50    --  105.75 133.00-153.00   50
 11  \w    -57.00  22.00   0.50    0.40    --  -50.29  19.00 120.00  158
 12  \w    -49.00  22.00   0.50    0.40    --  -50.29  57.00-150.00  142
 13  \w   -123.00 -59.00   0.50    0.40    --  -50.29 -37.00 120.00  128
 14  \w   -118.00 -67.00   0.50    0.40    --  -50.29 -57.00 -30.00  102
 15  \w   -114.00 -80.00   0.50    0.40    --  -50.29-125.00-180.00   68
 16  \w     39.00  92.00   0.50    1.50    --  105.75 -77.00  30.00  106
 17  \w     98.00 168.00   0.50    1.50    --  105.75  37.00-150.00  140
 18  \w     33.00 112.00   0.50    1.50    --  105.75 -37.00  90.00  158
 19  \w     83.00 108.00   0.50    1.50    --  105.75-110.00 -32.64   50
 20  \w     57.00 105.00   0.50    1.50    --  105.75 -99.00  30.00   96
 21  \w    101.00 177.00   0.50    1.50    --  105.75  19.00 -90.00  152
 22  \w     34.00 112.00   0.50    1.50    --  105.75 -37.00 -90.00  156
 23  \w     71.00 106.00   0.50    1.50    --  105.75 -99.00-150.00   70
 24  \w     48.00  92.00   0.50    1.50    --  105.75 -19.00  30.00   88
 25  \w     45.00 113.00   0.50    1.50    --  105.75 -19.00 150.00  136
 26  \w     34.00  92.00   0.50    1.50    --  105.75 -57.00 120.00  116
 27  \w     58.00 126.00   0.50    1.50    --  105.75 -77.00 120.00  136
 28  \w     37.00  90.00   0.50    1.50    --  105.75 -99.00 -60.00  106
 29  \w     35.00 112.00   0.50    1.50    --  105.75 -19.00 -90.00  154
 30  \w     39.00  65.00   0.50    1.50    --  105.75-125.00 120.00   52
 31  \w    104.00 131.00   0.50    1.50    --  105.75  19.00 -30.00   54
;
_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      0.0299467000
_diffrn_orient_matrix_UB_12      0.0429668000
_diffrn_orient_matrix_UB_13      0.0923293000
_diffrn_orient_matrix_UB_21      0.1062257000
_diffrn_orient_matrix_UB_22      0.0574259000
_diffrn_orient_matrix_UB_23      -0.0120849000
_diffrn_orient_matrix_UB_31      -0.0547717000
_diffrn_orient_matrix_UB_32      0.0882091000
_diffrn_orient_matrix_UB_33      0.0012190000
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36432
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.988
_diffrn_reflns_theta_min         3.535
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71825
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_preparation
'[(tBuPONOP)ReBr(CO)2] + Na[BarF4] in 1,2-difluorobenzene'
_exptl_crystal_recrystallization_method
'CH2Cl2 solution layered with hexane at room temperature.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.796
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         12178
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0659P)^2^+5.2978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11820
_reflns_number_total             12178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03201a2.cif
_cod_data_source_block           asw22138
_cod_original_cell_volume        3015.62(6)
_cod_database_code               7132003
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Re1 P2 B1 C40 F24 H40 N1 O4'
_chemical_oxdiff_usercomment     'JG091 - DCM/hex'
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.339
_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-F4 \\sim C31-F5 \\sim C31-F4A \\sim C31-F6A \\sim C31-F5A
 with sigma of 0.02
 C47-C44 \\sim C47A-C44
 with sigma of 0.02
 F16A-C47 \\sim F16A-C47A
 with sigma of 0.02
 F22-F23 \\sim F22-F24 \\sim F23-F24
 with sigma of 0.04
 C55-F22 \\sim C55-F23 \\sim C55-F24
 with sigma of 0.02
 C39-F10 \\sim C39-F10A \\sim C39-F12A \\sim C39-F11A \\sim C39-F12 \\sim
C39-F11
 with sigma of 0.02
 F6-F4 \\sim F6-F5 \\sim F4-F5 \\sim F4A-F6A \\sim F4A-F5A \\sim F6A-F5A
 with sigma of 0.04
 F18A-F16A \\sim F18A-F17A \\sim F16A-F17A
 with sigma of 0.04
 F10-F12 \\sim F10-F11 \\sim F10A-F12A \\sim F10A-F11A \\sim F12A-F11A \\sim
F12-F11
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C47 \\sim C47A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
4. Rigid body (RIGU) restrains
 C47A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(F4A)=Sof(F6A)=Sof(F5A)=1-FVAR(1)
 Sof(F6)=Sof(F4)=Sof(F5)=FVAR(1)
 Sof(F10A)=Sof(F12A)=Sof(F11A)=1-FVAR(2)
 Sof(F10)=Sof(F12)=Sof(F11)=FVAR(2)
 Sof(C47A)=Sof(F17B)=Sof(F18B)=1-FVAR(3)
 Sof(C47)=Sof(F18A)=Sof(F17A)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C49(H49), C35(H35), C41(H41), C27(H27), C33(H33), C43(H43),
 C12(H12), C29(H29), C53(H53), C51(H51), C37(H37), C14(H14), C13(H13), C45(H45)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C21(H21A,
 H21B,H21C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              19278
_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.768