Iron and Manganese Complexes of 2-Carbonyl Pyrrolyls: Scorpionate Sandwich Anions and Extended Structures
Li, Lihong; Clarkson, Guy J.; Lees, Martin R.; Howson, Suzanne E.; Tan, Sze-yin; Turner, Scott S.; Scott, Peter; Organometallics 34 (2015) 2543–; doi:10.1021/om501218a

data_4085768
_publ_section_title
;
 Iron and Manganese Complexes of 2-Carbonyl Pyrrolyls: Scorpionate
 Sandwich Anions and Extended Structures
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2543
_journal_paper_doi               10.1021/om501218a
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C32 H24 Mn N7 Na O3, C H1.50 N0.50'
_chemical_formula_sum            'C33 H25.5 Mn N7.5 Na O3'
_chemical_formula_weight         653.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.489(4)
_cell_angle_beta                 80.865(4)
_cell_angle_gamma                80.113(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3060(4)
_cell_length_b                   12.9626(4)
_cell_length_c                   13.0826(6)
_cell_measurement_reflns_used    9006
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.44
_cell_measurement_theta_min      3.79
_cell_volume                     1534.03(12)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15296
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         71.28
_diffrn_reflns_theta_min         3.79
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    4.033
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.1244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                5476
_reflns_number_total             5867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501218a_si_002.cif
_cod_data_source_block           ll31_[Na(CH3CN)2][(MnL33)Na(L33Mn)]
_cod_depositor_comments
;
Adding full bibliography for 4085764--4085769.cif.

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1534.05(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_moiety     '2(C32 H24 Mn N7 Na O3), 2(C H1.50 N0.50)'
_cod_original_formula_sum        'C66 H51 Mn2 N15 Na2 O6'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1306.08
_cod_database_code               4085768