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_7060455
_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, 2(C12 H10 N2 O2), C8 H4 O4, 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           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 117.498(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9837(13)
_cell_length_b                   6.9704(3)
_cell_length_c                   24.5066(13)
_cell_measurement_reflns_used    4824
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.1910
_cell_measurement_theta_min      3.8190
_cell_volume                     3482.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -35.00  31.00   1.00    3.05    --   22.39 -77.00 -30.00   66
  2  \w    -25.00  64.00   1.00    3.05    --   22.39 -99.00 -60.00   89
  3  \w    -21.00  63.00   1.00    3.05    --   22.39 -99.00  60.00   84
  4  \w     60.00  86.00   1.00    3.05    --   22.39  57.00  90.00   26
  5  \w      6.00  80.00   1.00    3.05    --   22.39  77.00 120.00   74
  6  \w    -40.00  31.00   1.00    3.05    --   22.39 -57.00-180.00   71
  7  \w    -42.00   0.00   1.00    3.05    --  -22.71 -77.00-180.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0294
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16719
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.591
_diffrn_reflns_theta_min         3.749
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67484
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4944
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0365P)^2^+2.9951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3865
_reflns_number_total             4944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj06279k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7060454--7060456.cif.'
_cod_database_code               7060455
_shelx_shelxl_version_number     2018/3
_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
 O002-H00C = O002-H00D
 0.85 with sigma of 0.02
 H00C-H00D
 1.34 with sigma of 0.04
 Mn01-H00E \\sim Mn01-H00F
 with sigma of 0.02
 Mn01-H00C \\sim Mn01-H00D
 with sigma of 0.02
3.a Free rotating group:
 O003(H00E,H00F), O00A(H00S,H00T)
3.b Rotating group:
 O004(H00G,H00H)
3.c Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B)
3.d Aromatic/amide H refined with riding coordinates:
 C00C(H00I), C00G(H00M), C00J(H00J), C00K(H00K), C00L(H00L), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R)
;
_shelx_res_checksum              55005
_shelx_hkl_checksum              19529
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;