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_7702009
_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
'C72 H64 N16 O4 Zn4, 6(Cl O4), 1.25(H2 O), 5(C2 H3 N)'
_chemical_formula_sum            'C82 H81.5 Cl6 N21 O29.25 Zn4'
_chemical_formula_weight         2303.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 92.979(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7902(5)
_cell_length_b                   22.1991(4)
_cell_length_c                   27.0999(7)
_cell_measurement_reflns_used    19610
_cell_measurement_temperature    285.93(10)
_cell_measurement_theta_max      73.0760
_cell_measurement_theta_min      3.0090
_cell_volume                     10087.2(4)
_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      285.93(10)
_diffrn_detector_area_resol_mean 21.3001
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0536717000
_diffrn_orient_matrix_UB_12      0.0200407000
_diffrn_orient_matrix_UB_13      0.0414423000
_diffrn_orient_matrix_UB_21      -0.0661621000
_diffrn_orient_matrix_UB_22      0.0171608000
_diffrn_orient_matrix_UB_23      -0.0389550000
_diffrn_orient_matrix_UB_31      -0.0343330000
_diffrn_orient_matrix_UB_32      -0.0641980000
_diffrn_orient_matrix_UB_33      0.0024582000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            57739
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.010
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63725
_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    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.775
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1431
_refine_ls_number_reflns         19796
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0776
_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^)+(0.1656P)^2^+14.4458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15288
_reflns_number_total             19796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01416b2.cif
_cod_data_source_block           4
_cod_database_code               7702009
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         c17h20n6o4cl1zn1
_reflns_odcompleteness_completeness 99.80
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N102, C103, C104
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C109: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C112: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C104 \\sim C103 \\sim N102: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O43) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O38) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{Cl16, O17, O18, O19, O20}
as
{Cl34, O35, O36, O37, O38}
{C94, C95}
as
{C103, C104}
5. Others
 Sof(O24)=Sof(O25)=Sof(O27)=1-FVAR(1)
 Sof(O22)=Sof(O23)=Sof(O26)=FVAR(1)
 Sof(N93)=Sof(C94)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=1-FVAR(2)
 Sof(N102)=Sof(C103)=Sof(C104)=Sof(H10G)=Sof(H10H)=Sof(H10I)=FVAR(2)
 Sof(H50C)=Sof(H50D)=Sof(H52C)=Sof(H52D)=Sof(C52A)=Sof(H52E)=Sof(H52F)=1-FVAR(3)
 Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H52A)=Sof(H52B)=FVAR(3)
 Fixed Sof: Cl34(0.25) O35(0.25) O36(0.25) O37(0.25) O38(0.25) Cl29(0.75)
 O30(0.75) O31(0.75) O32(0.75) O33(0.75) O44(0.25) N108(0.5) C109(0.5)
 C110(0.5) H11A(0.5) H11B(0.5) H11C(0.5) N105(0.75) C106(0.75) C107(0.75)
 H10A(0.75) H10B(0.75) H10C(0.75) N111(0.75) C112(0.75) C113(0.75) H11D(0.75)
 H11E(0.75) H11F(0.75)
6.a Riding coordinates:
 C104(H10G,H10H,H10I)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C49(H49A,H49B), C50(H50A,H50B),
 C50(H50C,H50D), C51A(H51A,H51B), C52(H52A,H52B), C52(H52C,H52D), C52A(H52E,
 H52F), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
 C22(H22), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
  C44(H44), C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C64(H64),
 C65(H65), C66(H66), C79(H79), C80(H80), C81(H81), C82(H82), C85(H85), C86(H86),
  C87(H87), C88(H88)
6.d Idealised Me refined with riding coordinates:
 C95(H95A,H95B,H95C)
6.e Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C107(H10A,H10B,H10C), C98(H98A,H98B,H98C), C113(H11D,
 H11E,H11F), C101(H10D,H10E,H10F)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'