Structural control: can [2 ×2] silver grids be formed from 4,5-disubstituted 3,6-di(2-pyridyl) pyridazines?
Bodman, Samantha E.; Crowther, Anthony C.; Geraghty, Paul B.; Fitchett, Christopher M.; CrystEngComm 17 (2015) 81–; doi:10.1039/C4CE01851F

data_7235427
_publ_section_title
;
 Structural control: can [2 \\times 2] silver grids be formed from
 4,5-disubstituted 3,6-di(2-pyridyl) pyridazines?
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              81
_journal_paper_doi               10.1039/C4CE01851F
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'2(C34 H28 Ag2 N8), 2(C H2 Cl2), 4(B F4), H2 O'
_chemical_formula_sum            'C70 H62 Ag4 B4 Cl4 F16 N16 O'
_chemical_formula_weight         2063.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.5639(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.76695(15)
_cell_length_b                   13.12396(9)
_cell_length_c                   25.09710(17)
_cell_measurement_reflns_used    35616
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.7774
_cell_measurement_theta_min      2.8920
_cell_volume                     7640.75(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -78.00   -1.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218  124.0000  117.0000 77

  2 omega   65.00  132.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -147.0000 -126.0000 67

  3 omega   30.00   56.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    9.0000  118.0000 26

  4 omega   88.00  177.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    9.0000  118.0000 89

  5 omega   81.00  157.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  147.0000  103.0000 76

  6 omega  -43.00   34.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218   37.0000  120.0000 77

  7 omega -111.00  -86.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218 -147.0000 -103.0000 25

  8 omega  -32.00    4.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218   37.0000 -180.0000 36

  9 omega  -28.00   36.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218   37.0000   60.0000 64

 10 omega   58.00   94.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -       39.9218 -125.0000    0.0000 36

 11 omega   72.00  148.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000 -120.0000 76

 12 omega  107.00  178.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  -30.0000 71

 13 omega   38.00  111.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   60.0000 73

 14 omega   29.00   90.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000   90.0000 61

 15 omega  117.00  166.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  124.0000  -38.0000 49

 16 omega   77.00  116.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 39

 17 omega   38.00   88.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 50

 18 omega   32.00   58.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 26

 19 omega   79.00  105.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 26

 20 omega   29.00   89.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -90.0000 60

 21 omega   63.00   88.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 25

 22 omega   72.00   98.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 26

 23 omega -114.00  -10.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218  -57.0000   90.0000 104

 24 omega -114.00  -10.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218  -57.0000  -30.0000 104

 25 omega -114.00  -10.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -      -39.9218  -57.0000 -150.0000 104

 26 omega    1.00   29.00   1.0000    6.1800
omega____ theta____ kappa____ phi______ frames
    -       39.9218   91.0000   13.0000 28

 27 omega   34.00   91.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 57

 28 omega   84.00  178.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -180.0000 94

 29 omega   81.00  178.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -120.0000 97

 30 omega   78.00  164.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 86

 31 omega   82.00  178.00   1.0000   24.7000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -90.0000 96
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0646012000
_diffrn_orient_matrix_UB_12      0.0236606000
_diffrn_orient_matrix_UB_13      0.0062609000
_diffrn_orient_matrix_UB_21      0.0125710000
_diffrn_orient_matrix_UB_22      -0.1145780000
_diffrn_orient_matrix_UB_23      -0.0039534000
_diffrn_orient_matrix_UB_31      -0.0088825000
_diffrn_orient_matrix_UB_32      0.0095807000
_diffrn_orient_matrix_UB_33      -0.0624552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            81531
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.966
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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    1.794
_exptl_crystal_description       block
_exptl_crystal_F_000             4013
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.604
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         15848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0744P)^2^+28.9034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13529
_reflns_number_total             15848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce01851f1.cif
_cod_data_source_block           6
_cod_original_cell_volume        7640.74(9)
_cod_database_code               7235427
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C17H14N4B1F4AG1
_chemical_oxdiff_usercomment     7490
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Others
 Sof(Ag7)=1-FVAR(1)
 Sof(Ag5)=Sof(Ag9)=0.5*(1-FVAR(2))
 Sof(Ag4)=Sof(Ag8)=0.5*FVAR(2)
 Sof(Ag6)=FVAR(1)
 Sof(F24)=1-FVAR(2)
 Sof(F21)=FVAR(2)
 Sof(F28)=1-FVAR(3)
 Sof(F30)=FVAR(3)
3.a Free rotating group:
 O93(H93A,H93B)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), C87(H87A,H87B), C90(H90A,H90B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
 C22(H22), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42),
  C43(H43), C56(H56), C57(H57), C58(H58), C59(H59), C62(H62), C63(H63),
 C64(H64), C65(H65), C77(H77), C78(H78), C79(H79), C80(H80), C83(H83), C84(H84),
  C85(H85), C86(H86)
;