Conformational control of the self-assembly of triple helicates and [2 × 2]-grids from zinc(II) and 3,6-di(2-pyridyl)pyridazine based ligands.
Bodman, Samantha E.; Fitchett, Christopher M.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12606–12613; doi:10.1039/c4dt01416b

data_7702005
_publ_section_title
;
 Conformational control of the self-assembly of triple helicates and [2
 \\times 2]-grids from zinc(II) and 3,6-di(2-pyridyl)pyridazine based
 ligands.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12606
_journal_page_last               12613
_journal_paper_doi               10.1039/c4dt01416b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C42 H30 N12 Zn2, 4(Cl O4), 4(C2 H3 N)'
_chemical_formula_sum            'C50 H42 Cl4 N16 O16 Zn2'
_chemical_formula_weight         1395.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8564(8)
_cell_length_b                   18.7724(6)
_cell_length_c                   12.3412(3)
_cell_measurement_reflns_used    13966
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      34.8470
_cell_measurement_theta_min      3.1770
_cell_volume                     5758.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      120.02(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0009981000
_diffrn_orient_matrix_UB_12      -0.0335803000
_diffrn_orient_matrix_UB_13      0.0263248000
_diffrn_orient_matrix_UB_21      -0.0270322000
_diffrn_orient_matrix_UB_22      0.0065973000
_diffrn_orient_matrix_UB_23      0.0153601000
_diffrn_orient_matrix_UB_31      -0.0090584000
_diffrn_orient_matrix_UB_32      -0.0160410000
_diffrn_orient_matrix_UB_33      -0.0487292000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81604
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.917
_diffrn_reflns_theta_min         2.687
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 7454 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         27996
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0415P)^2^+6.6125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.828
_reflns_number_gt                21167
_reflns_number_total             27996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01416b2.cif
_cod_data_source_block           1
_cod_database_code               7702005
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         c14h10n4o8cl2zn1
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_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
2. Shared sites
{C67A, C68B}
3. Uiso/Uaniso restraints and constraints
Uanis(O17B) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C67A) = Uanis(C68B)
4. Others
 Sof(C70A)=Sof(C71A)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(N69A)=1-FVAR(1)
 Sof(C70B)=Sof(C71B)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(N69B)=FVAR(1)
 Sof(Cl16)=Sof(O11)=Sof(O17B)=Sof(O18B)=1-FVAR(2)
 Sof(Cl16)=Sof(O17A)=Sof(O19A)=Sof(O20A)=FVAR(2)
 Sof(C67A)=Sof(C68A)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(N66A)=1-FVAR(3)
 Sof(C67B)=Sof(C68B)=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(N66B)=FVAR(3)
5.a Riding coordinates:
 C68B(H68D,H68E,H68F)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C18(H18), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C30(H30),
  C33(H33), C34(H34), C35(H35), C36(H36), C40(H40), C41(H41), C45(H45),
 C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C68A(H68A,H68B,H68C), C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C71A(H71A,
 H71B,H71C), C71B(H71D,H71E,H71F)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'