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_7060456
_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
'2(H6 Mn0.5 O3), C6 H2 O4 S, 2(C12 H10 N2 O2), 3(H2 O)'
_chemical_formula_sum            'C30 H40 Mn N4 O17 S'
_chemical_formula_weight         815.66
_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   mixed
_audit_creation_date             2021-02-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.02.06 svn.rb'dbe4f857' for OlexSys, GUI svn.r6224)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                87.899(3)
_cell_angle_beta                 84.516(3)
_cell_angle_gamma                77.151(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9616(10)
_cell_length_b                   11.8671(17)
_cell_length_c                   22.471(3)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      2.65
_cell_volume                     1801.4(4)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23796
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.274
_diffrn_reflns_theta_min         3.013
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0504 after correction.
The Ratio of minimum to maximum transmission is 0.7751.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         8845
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.9015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7178
_reflns_number_total             8845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj06279k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060454--7060456.cif.'
_cod_original_cell_volume        1801.5(4)
_cod_database_code               7060456
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.863
_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,H) groups
2. Restrained distances
 O12-H12A = O12-H12B
 0.85 with sigma of 0.02
 O13-H13A = O13-H13B
 0.85 with sigma of 0.02
 O14-H14C = O14-H14D
 0.85 with sigma of 0.02
 O9-H9A = O9-H9B
 0.85 with sigma of 0.02
 O11-H11A = O11-H11B
 0.85 with sigma of 0.02
 O10-H10A = O10-H10B
 0.85 with sigma of 0.02
 H11A-H11B
 1.34 with sigma of 0.04
 H12A-H12B
 1.34 with sigma of 0.04
 H14C-H14D
 1.34 with sigma of 0.04
 H13A-H13B
 1.34 with sigma of 0.04
 H9A-H9B
 1.34 with sigma of 0.04
 H10A-H10B
 1.34 with sigma of 0.04
 Mn1-H11A \\sim Mn1-H11B
 with sigma of 0.02
 Mn1-H9A \\sim Mn1-H9B
 with sigma of 0.02
 Mn1-H10A \\sim Mn1-H10B
 with sigma of 0.02
 Mn3-H12A \\sim Mn3-H12B
 with sigma of 0.02
 Mn3-H13A \\sim Mn3-H13B
 with sigma of 0.02
 Mn3-H14C \\sim Mn3-H14D
 with sigma of 0.02
3.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C22(H22), C27(H27), C21(H21), C17(H17), C23(H23), C15(H15),
 C16(H16), C24(H24), C18(H18), C10(H10), C9(H9), C11(H11), C12(H12), C6(H6),
 C3(H3), C5(H5), C4(H4)
;
_shelx_res_checksum              92146
_shelx_hkl_checksum              95520
_olex2_submission_special_instructions 'No special instructions were received'