The impact of metal ions on photoinduced electron-transfer properties: four photochromic metal‒organic frameworks based on a naphthalenediimide chromophore
Xu, Hui-Ling; Zeng, Xiao-Shan; Li, Jie; Xu, Yu-Ci; Qiu, Hai-Jiang; Xiao, Dong-Rong; CrystEngComm 20 (2018) 2430–; doi:10.1039/C8CE00213D

data_7230362
_publ_section_title
;
 The impact of metal ions on photoinduced electron-transfer properties:
 four photochromic metal--organic frameworks based on a naphthalenediimide
 chromophore
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2430
_journal_paper_doi               10.1039/C8CE00213D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C42 H38 Ca2 Cl N5 O15, C4 H9 N O'
_chemical_formula_sum            'C46 H47 Ca2 Cl N6 O16'
_chemical_formula_weight         1055.50
_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     iterative
_audit_creation_date             2017-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                63.933(2)
_cell_angle_beta                 78.652(7)
_cell_angle_gamma                86.531(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8893(9)
_cell_length_b                   16.7182(4)
_cell_length_c                   17.3044(4)
_cell_measurement_reflns_used    16875
_cell_measurement_temperature    291.87(10)
_cell_measurement_theta_max      72.8850
_cell_measurement_theta_min      4.5700
_cell_volume                     2518.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.87(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.996
_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   -106.00 -18.00   1.00    1.74    --  -37.03 -38.00 -90.00   88
  2  \w    -66.00  34.00   1.00    1.74    --  -37.03  19.00-180.00  100
  3  \w    -66.00  34.00   1.00    1.74    --  -37.03  19.00  90.00  100
  4  \w    -91.00  -3.00   1.00    1.74    --  -37.03 126.00  60.00   88
  5  \w     10.00 105.00   1.00    1.74    --   37.03  77.00 -90.00   95
  6  \w    -30.00  54.00   1.00    1.74    --   37.03 -57.00-120.00   84
  7  \w     20.00 104.00   1.00    1.74    --   37.03  57.00 -30.00   84
  8  \w      8.00 108.00   1.00    1.74    --   37.03  19.00-150.00  100
  9  \w      1.00  76.00   1.00    1.74    --   37.03 -99.00  90.00   75
 10  \w      1.00  76.00   1.00    1.74    --   37.03 -99.00  60.00   75
 11  \w     24.00  91.00   1.00    1.74    --   37.03-126.00  60.00   67
 12  \w     24.00  91.00   1.00    1.74    --   37.03-126.00-120.00   67
 13  \w      8.00  80.00   1.00    1.74    --   37.03-106.00-160.00   72
 14  \w     41.00 132.00   1.00    8.98    --  110.47 -30.00  30.00   91
 15  \w     41.00 109.00   1.00    8.98    --  110.47 -95.00 -60.00   68
 16  \w     44.00 129.00   1.00    8.98    --  110.47 -61.00-150.00   85
 17  \w     44.00 129.00   1.00    8.98    --  110.47 -61.00 -60.00   85
 18  \w     41.00 132.00   1.00    8.98    --  110.47 -30.00 120.00   91
 19  \w     89.00 178.00   1.00    8.98    --  110.47  30.00  90.00   89
 20  \w     41.00 116.00   1.00    8.98    --  110.47-112.00 120.00   75
 21  \w     44.00 129.00   1.00    8.98    --  110.47 -61.00 120.00   85
 22  \w     43.00 137.00   1.00    8.98    --  110.47 -77.00  30.00   94
 23  \w     93.00 178.00   1.00    8.98    --  110.47  45.00  60.00   85
 24  \w     41.00 116.00   1.00    8.98    --  110.47-112.00  60.00   75
 25  \w     40.00 149.00   1.00    8.98    --  110.47 -15.00-120.00  109
 26  \w     41.00 116.00   1.00    8.98    --  110.47-112.00-120.00   75
 27  \w     92.00 177.00   1.00    8.98    --  110.47  61.00 150.00   85
 28  \w   -104.00 -34.00   1.00    1.74    --  -37.03 -57.00 -90.00   70
 29  \w   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00 -90.00   95
 30  \w   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00-150.00   95
 31  \w   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00 120.00   95
 32  \w   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00  30.00   95
 33  \w   -107.00  -8.00   1.00    1.74    --  -37.03 -19.00 -60.00   99
 34  \w   -104.00 -20.00   1.00    1.74    --  -37.03 -57.00-120.00   84
 35  \w   -105.00 -10.00   1.00    1.74    --  -37.03 -77.00  60.00   95
 36  \w   -106.00 -18.00   1.00    1.74    --  -37.03 -38.00  90.00   88
 37  \w    -66.00  34.00   1.00    1.74    --  -37.03  19.00-150.00  100
 38  \w   -104.00 -20.00   1.00    1.74    --  -37.03 -57.00 150.00   84
 39  \w     10.00 105.00   1.00    1.74    --   37.03  77.00   0.00   95
 40  \w    -30.00  54.00   1.00    1.74    --   37.03 -57.00 -60.00   84
 41  \w     20.00 104.00   1.00    1.74    --   37.03  57.00  60.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0607989000
_diffrn_orient_matrix_UB_12      0.0944806000
_diffrn_orient_matrix_UB_13      -0.0325675000
_diffrn_orient_matrix_UB_21      0.0561759000
_diffrn_orient_matrix_UB_22      0.0028614000
_diffrn_orient_matrix_UB_23      -0.0907998000
_diffrn_orient_matrix_UB_31      -0.1357019000
_diffrn_orient_matrix_UB_32      0.0399711000
_diffrn_orient_matrix_UB_33      -0.0297362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34834
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         4.562
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.578
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8945
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1016P)^2^+2.6624P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7542
_reflns_number_total             8945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00213d2.cif
_cod_data_source_block           compound-4
_cod_depositor_comments
'Adding full bibliography for 7230359--7230362.cif.'
_cod_database_code               7230362
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C1 H1 O1 N1 Ca1'
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N6-C2
 1.57 with sigma of 0.01
 N4-C11
 1.57 with sigma of 0.01
 N3-C16
 1.47 with sigma of 0.01
 N3-C14
 1.57 with sigma of 0.01
 H14A-H13B
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N5) \\sim
Ueq, Uanis(C15) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C23(H23), C30(H30), C31(H31), C35(H35), C36(H36),
 C40(H40), C42(H42), C44(H44)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.574
_oxdiff_exptl_absorpt_empirical_full_min 0.667