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_7132004
_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 Br N O4 P2 Re'
_chemical_formula_sum            'C23 H39 Br N O4 P2 Re'
_chemical_formula_weight         721.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3315(2)
_cell_length_b                   10.26090(10)
_cell_length_c                   11.21410(10)
_cell_measurement_reflns_used    25416
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      76.5850
_cell_measurement_theta_min      3.6060
_cell_volume                     2799.75(4)
_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      110.05(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -116.00 -65.00   0.50    1.00    --  -48.70-140.00-140.00  102
  2  \w    -96.00 -56.00   0.50    1.00    --  -48.70 140.00 -80.00   80
  3  \w    -86.00 -26.00   0.50    1.00    --  -48.70 130.00 105.00  120
  4  \w   -118.00 -93.00   0.50    1.00    --  -48.70-130.00  33.00   50
  5  \w     49.00  86.00   0.50    1.00    --   48.70-140.00-140.00   74
  6  \w     37.00  69.00   0.50    1.00    --   48.70-130.00  33.00   64
  7  \w    111.00 136.00   0.50    3.00    --  107.75 130.00 105.00   50
  8  \w     52.00  77.00   0.50    3.00    --  107.75-130.00  33.00   50
  9  \w     83.00 108.00   0.50    3.00    --  107.75-140.00-140.00   50
 10  \w    107.00 137.00   0.50    3.00    --  107.75 140.00 -80.00   60
 11  \w   -118.00 -74.00   0.50    1.00    --  -48.70-125.00  60.00   88
 12  \w   -118.00 -79.00   0.50    1.00    --  -48.70-125.00 -90.00   78
 13  \w   -116.00 -73.00   0.50    1.00    --  -48.70-125.00-120.00   86
 14  \w   -120.00 -48.00   0.50    1.00    --  -48.70 -77.00-120.00  144
 15  \w   -114.00 -44.00   0.50    1.00    --  -48.70 -77.00 -60.00  140
 16  \w     64.00 115.00   0.50    1.00    --   48.70  57.00-120.00  102
 17  \w     35.00 121.00   0.50    3.00    --  107.75 -57.00   0.00  172
 18  \w     38.00 112.00   0.50    3.00    --  107.75-125.00-180.00  148
 19  \w     68.00 117.00   0.50    3.00    --  107.75 -37.00   0.00   98
 20  \w    150.00 175.00   0.50    3.00    --  107.75  37.00-180.00   50
 21  \w     95.00 146.00   0.50    3.00    --  107.75  37.00-180.00  102
 22  \w     33.00 120.00   0.50    3.00    --  107.75 -19.00-120.00  174
 23  \w    141.00 177.00   0.50    3.00    --  107.75 125.00  60.00   72
 24  \w     83.00 109.00   0.50    3.00    --  107.75-125.00  60.00   52
 25  \w     40.00 103.00   0.50    3.00    --  107.75 -99.00-120.00  126
 26  \w     97.00 178.00   0.50    3.00    --  107.75  19.00 120.00  162
 27  \w     41.00 106.00   0.50    3.00    --  107.75 -99.00 150.00  130
 28  \w    114.00 166.00   0.50    3.00    --  107.75  19.00   0.00  104
 29  \w     37.00  76.00   0.50    3.00    --  107.75 -99.00-150.00   78
 30  \w     37.00 106.00   0.50    3.00    --  107.75 -99.00 -30.00  138
 31  \w     44.00 105.00   0.50    3.00    --  107.75 -99.00  30.00  122
 32  \w    123.00 149.00   0.50    3.00    --  107.75  37.00 -90.00   52
 33  \w     35.00 109.00   0.50    3.00    --  107.75 -57.00-180.00  148
 34  \w    112.00 177.00   0.50    3.00    --  107.75  19.00  60.00  130
;
_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      -0.0223845000
_diffrn_orient_matrix_UB_12      -0.0368337000
_diffrn_orient_matrix_UB_13      -0.1240376000
_diffrn_orient_matrix_UB_21      -0.0591871000
_diffrn_orient_matrix_UB_22      0.0187948000
_diffrn_orient_matrix_UB_23      0.0456086000
_diffrn_orient_matrix_UB_31      0.0020027000
_diffrn_orient_matrix_UB_32      0.1443226000
_diffrn_orient_matrix_UB_33      -0.0375832000
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32476
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.931
_diffrn_reflns_theta_min         3.633
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42571
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_recrystallization_method 'toluene/hexane -30C'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 2513 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5693
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0320P)^2^+3.6465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                5609
_reflns_number_total             5693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03201a2.cif
_cod_data_source_block           asw22124
_cod_database_code               7132004
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H31 Re1 P2 N1 O4 Br1'
_chemical_oxdiff_usercomment     'JG082 - toluene/hex -30C'
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.178
_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:
 C12(H12), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C19(H19A,H19B,H19C),
 C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C),
 C21(H21A,H21B,H21C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              71698
_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 2.500
_oxdiff_exptl_absorpt_empirical_full_min 0.684