Bipyridine based metallogels: an unprecedented difference in photochemical and chemical reduction in the in situ nanoparticle formation.
Tatikonda, Rajendhraprasad; Bertula, Kia; Nonappa, ?; Hietala, Sami; Rissanen, Kari; Haukka, Matti; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2793–2802; doi:10.1039/c6dt04253h

data_7041926
_publ_section_title
;
 Bipyridine based metallogels: an unprecedented difference in
 photochemical and chemical reduction in the in situ nanoparticle
 formation.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2793
_journal_page_last               2802
_journal_paper_doi               10.1039/c6dt04253h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         '2(C11 H9 N2 O)'
_chemical_formula_sum            'C22 H18 N4 O2'
_chemical_formula_weight         370.40
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-23 deposited with the CCDC.
2017-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                114.646(6)
_cell_angle_beta                 103.516(5)
_cell_angle_gamma                93.852(5)
_cell_formula_units_Z            2
_cell_length_a                   6.2801(4)
_cell_length_b                   12.0904(8)
_cell_length_c                   13.3168(8)
_cell_measurement_reflns_used    5160
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.7750
_cell_measurement_theta_min      3.8970
_cell_volume                     877.92(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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    -47.00  47.00   1.00   30.00    --  -18.14  77.00-120.00   94
  2  \w    -37.00  54.00   1.00   30.00    --  -18.14  37.00  30.00   91
  3  \w    -83.00  -9.00   1.00   30.00    --  -18.14 137.00  27.90   74
  4  \w     -2.00  88.00   1.00   30.00    --   19.23  57.00 -90.00   90
  5  \w    -50.00  41.00   1.00   30.00    --   19.23 -57.00 120.00   91
  6  \w     10.00  61.00   1.00   30.00    --   19.23 -99.00 -60.00   51
  7  \w     -2.00  88.00   1.00   30.00    --   19.23  57.00  30.00   90
  8  \w    -10.00  87.00   1.00   30.00    --   19.23  77.00 120.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0078966000
_diffrn_orient_matrix_UB_12      -0.0627688000
_diffrn_orient_matrix_UB_13      -0.0101131000
_diffrn_orient_matrix_UB_21      -0.0843059000
_diffrn_orient_matrix_UB_22      0.0065729000
_diffrn_orient_matrix_UB_23      0.0283404000
_diffrn_orient_matrix_UB_31      -0.0825145000
_diffrn_orient_matrix_UB_32      -0.0182458000
_diffrn_orient_matrix_UB_33      -0.0532993000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11863
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.4698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                3201
_reflns_number_total             3787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04253h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7041926--7041928.cif.'
_cod_original_cell_volume        877.92(10)
_cod_database_code               7041926
_chemical_oxdiff_formula         'C11 H18 N4 O2 '
_chemical_oxdiff_usercomment     'Clear, Colorless, Block'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C6(H6A,H6B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C13(H13), C22(H22), C15(H15), C4(H4), C20(H20), C8(H8), C5(H5),
 C9(H9), C21(H21), C11(H11), C19(H19), C16(H16), C10(H10)
;
_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 1.148
_oxdiff_exptl_absorpt_empirical_full_min 0.921