Three Mn‒viologen complexes containing 1-carboxyethyl-4,4′-bipyridinium: crystal structures, photochromism and theoretical calculations
Zhao, Guozheng; Liu, Wenya; Yuan, Fang; Liu, Jinjian; New Journal of Chemistry 45 (2021) 6787–6795; doi:10.1039/D0NJ06279K

data_7060454
_publ_section_title
;
 Three Mn--viologen complexes containing
 1-carboxyethyl-4,4&#x2032;-bipyridinium: crystal structures,
 photochromism and theoretical calculations
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6787
_journal_page_last               6795
_journal_paper_doi               10.1039/D0NJ06279K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety
'H12 Mn O6, 1.176(C6.8 H3.4 O3.4), 2(C12 H10 N2 O2), 2(H2 O)'
_chemical_formula_sum            'C32 H40 Mn N4 O16'
_chemical_formula_weight         791.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.02.10 svn.rb'16c95d35' for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3426(7)
_cell_length_b                   6.9034(4)
_cell_length_c                   20.5241(11)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      3.11
_cell_volume                     1747.01(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22675
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_min         2.951
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5527
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             826
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4327
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+1.7755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3893
_reflns_number_total             4327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj06279k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7060454--7060456.cif.'
_cod_database_code               7060454
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C26-C27 = C27-C26_$1 = C26-C25 = C25_$1-C24 = C24-C25 = C25-C26
 1.39 with sigma of 0.01
 C14-C16 = C16-C17 = C17-C16_$1 = C16-C14 = C14_$1-C15 = C15-C14
 1.39 with sigma of 0.01
 C14-C17 \\sim C16-C16_$1 \\sim C17-C14_$1 \\sim C16_$1-C15 \\sim C14_$1-C14
\\sim C15-C16
 with sigma of 0.02
 C26-C26_$1 \\sim C27-C25_$1 \\sim C26_$1-C24 \\sim C25_$1-C25 \\sim C24-C26
\\sim C25-C27
 with sigma of 0.02
3. Restrained planarity
 C26, C27, C26_$1, C25_$1, C24, C25
 with sigma of 0.1
 C14, C16, C17, C16_$1, C14_$1, C15
 with sigma of 0.1
4. Others
 Fixed Sof: O4(0.85) O1(0.85) O2(0.85) N1(0.85) O3(0.85) C3B(0.85) H3B(0.85)
 C14(0.85) C1(0.85) C5B(0.85) H5B(0.85) C13(0.85) C15(0.425) H15(0.425)
 C2(0.85) H2A(0.85) H2B(0.85) C6(0.85) H6(0.85) C16(0.85) H16(0.85) C4(0.85)
 H4(0.85) C17(0.425) H17(0.425) O19(0.15) C23(0.15) H23(0.15) C22(0.15)
 H22(0.15) N21(0.15) C18(0.15) C20(0.15) H20A(0.15) H20B(0.15) C28(0.15)
 O29(0.15) C24(0.075) H24(0.075) C25(0.15) H25(0.15) C27(0.075) H27(0.075)
 C26(0.15) O9(0.15) O10(0.15) C3A(0.15) H3A(0.15) C5A(0.15) H5A(0.15)
5.a Free rotating group:
 O8(H8A,H8B)
5.b Rotating group:
 O7(H7A,H7B), O5(H5C), O6(H6A,H6B)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C20(H20A,H20B)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C3B(H3B), C5B(H5B), C10(H10), C15(H15), C11(H11), C12(H12), C6(H6),
 C16(H16), C4(H4), C17(H17), C23(H23), C22(H22), C24(H24), C25(H25), C27(H27),
 C3A(H3A), C5A(H5A)
;
_shelx_res_checksum              3436
_shelx_hkl_checksum              13712
_olex2_submission_special_instructions 'No special instructions were received'