Crystallographic identification of a series of manganese porphyrin complexes with nitrogenous bases
Lahanas, Nicole; Kucheryavy, Pavel; Lalancette, Roger A.; Lockard, Jenny V.; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619001232

data_2021488
_publ_section_title
;
 Crystallographic identification of a series of manganese porphyrin
 complexes with nitrogenous bases
;
_journal_coeditor_code           JX3027
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619001232
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Mn (C44 H28 N4) (C6 H12 N2)] Cl, C6 H12 N2, C7 H8, 0.25H2 O'
_chemical_formula_moiety
'C50 H40 Cl Mn N6 +, Cl -, C6 H12 N2, C7 H8, 0.25(O)'
_chemical_formula_sum            'C63 H60 Cl Mn N8 O0.25'
_chemical_formula_weight         1023.58
_chemical_name_systematic
;
(1,4-Diazabicyclo[2.2.2]octane)(5,10,15,20-tetraphenylporphyrin)manganese(III)
chloride--1,4-diazabicyclo[2.2.2]octane--toluene--water (4/4/4/1)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_cell_angle_alpha                95.7740(10)
_cell_angle_beta                 92.1990(10)
_cell_angle_gamma                113.6300(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4402(2)
_cell_length_b                   13.4019(3)
_cell_length_c                   18.6407(4)
_cell_measurement_reflns_used    9495
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.56
_cell_measurement_theta_min      2.39
_cell_volume                     2595.35(9)
_computing_cell_refinement
;
APEX2 (Bruker, 2006)
;
_computing_data_collection
;
APEX2 (Bruker, 2006)
;
_computing_data_reduction
;
SAINT (Bruker, 2005)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker SMART CCD APEXII area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24215
_diffrn_reflns_theta_full        66.660
_diffrn_reflns_theta_max         66.660
_diffrn_reflns_theta_min         2.391
_exptl_absorpt_coefficient_mu    2.946
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.175
_refine_diff_density_max         1.300
_refine_diff_density_min         -0.680
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         8538
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0887P)^2^+3.2657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                6596
_reflns_number_total             8538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jx3027sup1.cif
_cod_data_source_block           IV_DABCO
_cod_database_code               2021488
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.627
_shelx_hkl_checksum              28065
_shelx_res_checksum              69437
_cod_database_fobs_code 2021488