Synthesis and crystal structures of manganese(I) carbonyl complexes bearing ester-substituted α-diimine ligands
Kanno, Takatoshi; Takase, Tsugiko; Oyama, Dai; Acta Crystallographica Section E 76 (2020) 1433–1436; doi:10.1107/S2056989020010750

data_2243531
_publ_section_title
;
 Synthesis and crystal structures of manganese(I) carbonyl complexes
 bearing ester-substituted \a-diimine ligands
;
_journal_coeditor_code           DJ2012
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1433
_journal_page_last               1436
_journal_paper_doi               10.1107/S2056989020010750
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Mn Br (C16 H16 N2 O4) (C O)3]'
_chemical_formula_moiety         'C19 H16 Br Mn N2 O7'
_chemical_formula_sum            'C19 H16 Br Mn N2 O7'
_chemical_formula_weight         519.19
_chemical_name_systematic
;
<i>fac</i>-Bromidotricarbonyl(diethyl
2,2'-bipyridine-4,4'-dicarboxylate-\k^2^<i>N</i>,<i>N</i>')manganese(I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.347(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.7054(7)
_cell_length_b                   13.9151(7)
_cell_length_c                   13.3273(8)
_cell_measurement_reflns_used    5049
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.22
_cell_volume                     2035.3(2)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020), ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2019), PLATON (Spek, 2020), publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20542
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         3.217
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.662
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4653
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0550P)^2^+1.4779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                4050
_reflns_number_total             4653
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            dj2012sup1.cif
_cod_data_source_block           I
_cod_database_code               2243531
_shelx_hkl_checksum              74360
_shelx_res_checksum              7794
_cod_database_fobs_code 2243531