Synthesis, spectroscopic and crystallographic characterization of various cymantrenyl thioethers [Mn{C<sub>5</sub>H<sub>x</sub>Br<sub>y</sub>(SMe)<sub>z</sub>}(PPh<sub>3</sub>)(CO)<sub>2</sub>].
Klein-Hessling, Christian; Blockhaus, Tobias; Sünkel, Karlheinz; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S205322962400603X

data_2312540
_publ_section_title
;
 Synthesis, spectroscopic and crystallographic characterization of various
 cymantrenyl thioethers
 [Mn{C<sub>5</sub>H<sub>x</sub>Br<sub>y</sub>(SMe)<sub>z</sub>}(PPh<sub>3</sub>)(CO)<sub>2</sub>].
;
_journal_coeditor_code           QF3063
_journal_issue                   8
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S205322962400603X
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac
'[Mn (C6 H6 S Br) (C18 H15 P) (C O)2], 0.75C6 H12'
_chemical_formula_moiety         '2(C26 H21 Br Mn O2 P S), 0.75(C6 H12)'
_chemical_formula_sum            'C56.5 H51 Br2 Mn2 O4 P2 S2'
_chemical_formula_weight         1189.73
_chemical_name_systematic
'Dicarbonyl[\h^5^-1-bromo-2-(methylsulfanyl)cyclopentadienyl](triphenylphosphane-\k<i>P</i>)manganese cyclohexane 0.75-solvate'
_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_method           SHELXL-2019/3
_cell_angle_alpha                87.692(2)
_cell_angle_beta                 82.138(2)
_cell_angle_gamma                62.507(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3309(5)
_cell_length_b                   10.7727(5)
_cell_length_c                   13.0821(6)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    108
_cell_measurement_theta_max      28.2881
_cell_measurement_theta_min      2.5614
_cell_volume                     1278.93(11)
_computing_cell_refinement
;
APEX2 (Bruker, 2011)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2011)
;
_computing_publication_material
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      108(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21220
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.309
_diffrn_reflns_theta_min         2.900
_diffrn_source                   'rotating anode generator'
_exptl_absorpt_coefficient_mu    2.247
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS2016; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         5.858
_refine_diff_density_min         -1.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6351
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0645P)^2^+9.2055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                5421
_reflns_number_total             6351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qf3063.cif
_cod_data_source_block           comp_2
_cod_original_formula_sum        'C56.50 H51 Br2 Mn2 O4 P2 S2'
_cod_database_code               2312540
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.956
_shelx_hkl_checksum              73765
_shelx_res_checksum              89082