Lone pair-π interaction-induced generation of photochromic coordination networks with photoswitchable conductance
Liao, Jian-Zhen; Chang, Jian-Fei; Meng, Lingyi; Zhang, Hai-Long; Wang, Sa-Sa; Lu, Can-Zhong; Chem. Commun.  (2017) –; doi:10.1039/C7CC05150F

data_7120516
_publ_section_title
;
 Lone pair-\p interaction-induced generation of photochromic coordination
 networks with photoswitchable conductance
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05150F
_journal_year                    2017
_chemical_formula_moiety         'C18 H12 N2 O10 S2 -2, 2(Na +), 4(H2 O)'
_chemical_formula_sum            'C18 H20 N2 Na2 O14 S2'
_chemical_formula_weight         598.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8364(2)
_cell_length_b                   11.9343(4)
_cell_length_c                   27.7283(9)
_cell_measurement_reflns_used    3067
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3560
_cell_measurement_theta_min      6.3690
_cell_volume                     2262.29(12)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -65.00   4.00   1.00    5.00    --  -42.45  38.00  90.00   69
  2  \w    -97.00 -39.00   1.00    5.00    --  -42.45   0.00-150.00   58
  3  \w      3.00  29.00   1.00    5.00    --  -42.45   0.00-150.00   26
  4  \w    118.00 178.00   1.00    5.00    --  106.62 125.00-180.00   60
  5  \w     21.00 138.00   1.00    5.00    --  106.62   0.00-180.00  117
  6  \w     27.00  65.00   1.00    5.00    --  106.62 -94.00 150.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0105843000
_diffrn_orient_matrix_UB_12      0.0458127000
_diffrn_orient_matrix_UB_13      0.0518780000
_diffrn_orient_matrix_UB_21      -0.0770075000
_diffrn_orient_matrix_UB_22      0.1126003000
_diffrn_orient_matrix_UB_23      -0.0193845000
_diffrn_orient_matrix_UB_31      -0.2115011000
_diffrn_orient_matrix_UB_32      -0.0433746000
_diffrn_orient_matrix_UB_33      0.0045779000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            4359
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         6.385
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66069
_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_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+1.2020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1869
_reflns_number_total             2002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc05150f2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;

2024-04-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C9 H10 N Na O7 S'
_cod_original_formula_weight         299.23
_cod_original_formula_moiety         'C9 H10 N Na O7 S'
_cod_original_formula_units_Z            8
_cod_database_code               7120516
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Na H C O S P N'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8)
;
_shelx_res_checksum              26183
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.586