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_7132001
_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_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-06-27 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                105.823(5)
_cell_angle_beta                 106.400(5)
_cell_angle_gamma                97.542(5)
_cell_formula_units_Z            2
_cell_length_a                   13.0245(6)
_cell_length_b                   14.1722(9)
_cell_length_c                   17.0849(12)
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      0.824
_cell_measurement_theta_min      0.046
_cell_volume                     2835.6(3)
_computing_cell_refinement       'DIALS (Winter et al., 2018)'
_computing_data_collection       EPU-D
_computing_data_reduction        'DIALS (Winter et al., 2018)'
_computing_molecular_graphics    'ShelXle (H\"ubschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      80(2)
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean 35.7
_diffrn_detector_type            'Thermo Scientific Ceta-D'
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       'electron microscope'
_diffrn_measurement_device_type  'Thermo Scientific Glacios'
_diffrn_measurement_method       'profile fitting from continuous rotation'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.1748
_diffrn_reflns_av_unetI/netI     0.1347
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43604
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.866
_diffrn_reflns_theta_min         0.046
_diffrn_source                   'electron microscope'
_diffrn_source_type              'Thermo Scientific Glacios'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'electron diffraction, unknown absorption'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       'nano crystals'
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.0010
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.0001
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       1920(23)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         9903
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1993
_refine_ls_R_factor_gt           0.1514
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1956P)^2^+1.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3830
_refine_ls_wR_factor_ref         0.4084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5780
_reflns_number_total             9903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03201a2.cif
_cod_data_source_block           JG064_a
_cod_database_code               7132001
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              52953