Distal scaffold flexibility accelerates ligand substitution kinetics in manganese(I) tricarbonyls: flexible thianthrene <i>versus</i> rigid anthracene scaffolds.
Labrecque, Jordan; Cho, Yae-In; McIntosh, Daniel K.; Agboola, Faridat; Rose, Michael J.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt04048d

data_7712528
_publ_section_title
;
 Distal scaffold flexibility accelerates ligand substitution kinetics in
 manganese(I) tricarbonyls: flexible thianthrene <i>versus</i> rigid
 anthracene scaffolds.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt04048d
_journal_year                    2023
_chemical_formula_moiety         'C22 H14 N2 S2, C H2 Cl2'
_chemical_formula_sum            'C23 H16 Cl2 N2 S2'
_chemical_formula_weight         455.40
_chemical_name_systematic        thianth-py2
_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_date             2019-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2023-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                77.276(2)
_cell_angle_beta                 88.191(2)
_cell_angle_gamma                83.065(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5739(2)
_cell_length_b                   11.5905(3)
_cell_length_c                   11.9375(3)
_cell_measurement_reflns_used    6090
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.5
_cell_measurement_theta_min      3.76
_cell_volume                     1014.71(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7859
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.633
_diffrn_reflns_theta_min         3.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.897
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       prism
_exptl_crystal_F_000             468
_exptl_crystal_recrystallization_method 'Vapor diffusion'
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+1.2750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3935
_reflns_number_total             4062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04048d2.cif
_cod_data_source_block           jhl-thiann2
_cod_original_cell_volume        1014.72(5)
_cod_database_code               7712528
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.508
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C23-Cl2 \\sim C23-Cl2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2) = Uanis(Cl2A)
4. Others
 Sof(H23C)=Sof(H23D)=Sof(Cl2A)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(Cl2)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C23(H23C,H23D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              94714
_shelx_hkl_checksum              75977
_olex2_submission_special_instructions 'No special instructions were received'