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_7702007
_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         'C51 H42 N12 Zn2, 4(Cl O4), 2.5(C2 H3 N)'
_chemical_formula_sum            'C56 H49.5 Cl4 N14.5 O16 Zn2'
_chemical_formula_weight         1454.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_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            8
_cell_length_a                   24.6982(3)
_cell_length_b                   22.0178(2)
_cell_length_c                   21.7705(4)
_cell_measurement_reflns_used    18841
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      73.5670
_cell_measurement_theta_min      3.3490
_cell_volume                     11838.8(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 0.984
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0583751000
_diffrn_orient_matrix_UB_12      -0.0244634500
_diffrn_orient_matrix_UB_13      -0.0036738500
_diffrn_orient_matrix_UB_21      0.0209335000
_diffrn_orient_matrix_UB_22      0.0647362500
_diffrn_orient_matrix_UB_23      -0.0124411500
_diffrn_orient_matrix_UB_31      0.0068451000
_diffrn_orient_matrix_UB_32      0.0102691000
_diffrn_orient_matrix_UB_33      0.0695528000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31222
_diffrn_reflns_point_group_measured_fraction_full 0.866
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.753
_diffrn_reflns_theta_min         3.369
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33109
_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    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             5944
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 3727 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         10099
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0598P)^2^+12.1345P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.741
_reflns_Friedel_fraction_max     0.710
_reflns_number_gt                9547
_reflns_number_total             10099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01416b2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_formula_sum        'C56 H49.50 Cl4 N14.50 O16 Zn2'
_cod_database_code               7702007
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 98.28
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H72A(0.5) H72B(0.5) H72C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C28(H28A,H28B), C9(H9A,H9B), C29(H29A,H29B), C7(H7A,H7B),
 C30(H30A,H30B), C50(H50A,H50B), C51(H51A,H51B), C49(H49A,H49B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C19(H19), C63(H63), C54(H54), C41(H41), C40(H40), C33(H33),
 C36(H36), C35(H35), C20(H20), C12(H12), C62(H62), C56(H56), C21(H21), C39(H39),
  C61(H61), C55(H55), C13(H13), C34(H34), C60(H60), C57(H57), C42(H42),
 C15(H15), C18(H18)
3.c Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C69(H69A,H69B,H69C), C66(H66A,H66B,H66C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'