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_7131999
_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         'C20 H31 Mn N O5 P2, C32 H12 B F24'
_chemical_formula_sum            'C52 H43 B F24 Mn N O5 P2'
_chemical_formula_weight         1345.56
_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                105.704(4)
_cell_angle_beta                 106.445(4)
_cell_angle_gamma                97.358(4)
_cell_formula_units_Z            2
_cell_length_a                   12.9543(6)
_cell_length_b                   14.1111(6)
_cell_length_c                   17.0692(8)
_cell_measurement_reflns_used    7808
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      70.9390
_cell_measurement_theta_min      5.2980
_cell_volume                     2809.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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    -15.00  28.00   1.00    1.00    --    0.00 -80.00 138.00   43
  2  \w    -21.00   4.00   1.00    1.00    --    0.00 -77.00-150.00   25
  3  \w    -62.00 -36.00   1.00    1.00    --    0.00 -38.00-150.00   26
  4  \w    -17.00  20.00   1.00    1.00    --    0.00 -38.00-150.00   37
  5  \w    -19.00  32.00   1.00    1.00    --    0.00  77.00   0.00   51
  6  \w     38.00 109.00   1.00    3.56    --   54.00-125.00 -60.00   71
  7  \w     33.00 124.00   1.00    3.56    --   54.00  38.00   0.00   91
  8  \w     33.00  64.00   1.00    3.56    --   54.00 -99.00   0.00   31
  9  \w     10.00 121.00   1.00    3.56    --   54.00  19.00 -60.00  111
 10  \w    -10.00  72.00   1.00    3.56    --   54.00 -57.00  30.00   82
 11  \w    -11.00  66.00   1.00    3.56    --   54.00 -57.00 120.00   77
 12  \w     66.00 108.00   1.00    3.56    --  108.00-111.00-180.00   42
 13  \w    117.00 143.00   1.00    3.56    --  108.00 111.00  90.00   26
 14  \w    105.00 176.00   1.00    3.56    --  108.00 111.00 -30.00   71
 15  \w     68.00  94.00   1.00    3.56    --  108.00 -91.00  90.00   26
 16  \w     61.00 109.00   1.00    3.56    --  108.00-111.00  90.00   48
 17  \w     75.00 129.00   1.00    3.56    --  108.00 178.00  30.00   54
 18  \w    115.00 177.00   1.00    3.56    --  108.00  77.00-150.00   62
 19  \w    104.00 177.00   1.00    3.56    --  108.00  77.00-180.00   73
 20  \w     42.00 107.00   1.00    3.56    --  108.00 -38.00 -90.00   65
 21  \w     41.00 130.00   1.00    3.56    --  108.00 -50.00  60.00   89
 22  \w    110.00 176.00   1.00    3.56    --  108.00  38.00  90.00   66
 23  \w     49.00 113.00   1.00    3.56    --  108.00 -25.00 150.00   64
 24  \w     39.00  81.00   1.00    3.56    --  108.00 -91.00  30.00   42
 25  \w     55.00  81.00   1.00    3.56    --  108.00-111.00 -90.00   26
 26  \w     82.00 109.00   1.00    3.56    --  108.00-111.00 -90.00   27
 27  \w     49.00 109.00   1.00    3.56    --  108.00-111.00   0.00   60
 28  \w     95.00 131.00   1.00    3.56    --  108.00 -77.00 150.00   36
 29  \w     84.00 169.00   1.00    3.56    --  108.00  38.00 150.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1054990000
_diffrn_orient_matrix_UB_12      0.0344216000
_diffrn_orient_matrix_UB_13      0.0796770000
_diffrn_orient_matrix_UB_21      -0.0289861000
_diffrn_orient_matrix_UB_22      0.1033356000
_diffrn_orient_matrix_UB_23      0.0298591000
_diffrn_orient_matrix_UB_31      -0.0648037000
_diffrn_orient_matrix_UB_32      -0.0407786000
_diffrn_orient_matrix_UB_33      0.0514263000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20116
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.137
_diffrn_reflns_theta_min         3.623
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_recrystallization_method
'CH2Cl2 solution layered with pentane at room temperature'
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         10626
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0525P)^2^+1.0996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9200
_reflns_number_total             10626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03201a2.cif
_cod_data_source_block           asw21085
_cod_database_code               7131999
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H43 B1 F24 Mn1 N1 O5 P2'
_chemical_oxdiff_usercomment     'Joe Goodall - JG031 150 K after 298 K'
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.548
_olex2_refinement_description
;
1. Restrained distances
 F21-F19 \\sim F21-F20 \\sim F19-F20 \\sim F21A-F19A \\sim F21A-F20A \\sim
F19A-F20A
 with sigma of 0.04
 F8-F9 \\sim F8-F7 \\sim F9A-F8A \\sim F9A-F7A \\sim F8A-F7A \\sim F9-F7
 with sigma of 0.04
 C35-F8 \\sim C35-F9A \\sim C35-F8A \\sim C35-F7A \\sim C35-F9 \\sim C35-F7
 with sigma of 0.02
 C34-F11 \\sim C34-F10 \\sim C34-F12
 with sigma of 0.02
 F10-F11 \\sim F10-F12 \\sim F11-F12
 with sigma of 0.04
 C42-F15 \\sim C42-F14 \\sim C42-F13 \\sim C42-F13A \\sim C42-F15A \\sim
C42-F14A \\sim C42-C38
 with sigma of 0.02
 C50-F21 \\sim C50-F19 \\sim C50-F20 \\sim C50-F21A \\sim C50-F19A \\sim
C50-F20A \\sim C50-C46
 with sigma of 0.02
 F15-F14 \\sim F15-F13 \\sim F14-F13 \\sim F13A-F15A \\sim F13A-F14A \\sim
F15A-F14A
 with sigma of 0.04
 F12-C34 \\sim F12A-C34A
 with sigma of 0.02
 F11-C34 \\sim F11A-C34A
 with sigma of 0.02
 C34-C30 \\sim C34A-C30
 with sigma of 0.02
 F10-C34 \\sim F10-C34A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F9 \\sim F9A \\sim F7 \\sim F7A \\sim F8 \\sim F8A: within 2A with sigma of
0.05 and sigma for terminal atoms of 0.01 within 2A
F10 \\sim F12 \\sim F11: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
3. Rigid body (RIGU) restrains
 F9, F9A, F7, F7A, F8, F8A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.001
 F10, F12, F11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F21A)=Sof(F19A)=Sof(F20A)=1-FVAR(1)
 Sof(F21)=Sof(F19)=Sof(F20)=FVAR(1)
 Sof(F13A)=Sof(F15A)=Sof(F14A)=1-FVAR(2)
 Sof(F15)=Sof(F14)=Sof(F13)=FVAR(2)
 Sof(F9A)=Sof(F8A)=Sof(F7A)=1-FVAR(3)
 Sof(F8)=Sof(F9)=Sof(F7)=FVAR(3)
 Sof(F12A)=Sof(C34A)=Sof(F11A)=1-FVAR(4)
 Sof(F11)=Sof(C34)=Sof(F12)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C4(H4), C13(H13), C10(H10)
5.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C33(H33), C22(H22), C24(H24), C37(H37), C47(H47), C29(H29),
 C49(H49), C31(H31), C41(H41), C45(H45), C39(H39), C17(H17), C19(H19), C18(H18)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              48446
_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 2.619
_oxdiff_exptl_absorpt_empirical_full_min 0.633