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_7702010
_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
'C76 H78 N16 O4 Zn4, 6(Cl O4), 1.5(H2 O), 0.5(C2 H5 N O), 5.5(C2 H3 N)'
_chemical_formula_sum            'C88 H102 Cl6 N22 O30 Zn4'
_chemical_formula_weight         2422.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                101.3748(11)
_cell_angle_beta                 95.3521(12)
_cell_angle_gamma                96.5500(11)
_cell_formula_units_Z            2
_cell_length_a                   14.0182(2)
_cell_length_b                   15.9372(2)
_cell_length_c                   24.4801(3)
_cell_measurement_reflns_used    32800
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.7420
_cell_measurement_theta_min      3.0490
_cell_volume                     5288.93(12)
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0173816000
_diffrn_orient_matrix_UB_12      0.0887846000
_diffrn_orient_matrix_UB_13      -0.0118601000
_diffrn_orient_matrix_UB_21      0.0972920000
_diffrn_orient_matrix_UB_22      0.0410400000
_diffrn_orient_matrix_UB_23      0.0347910000
_diffrn_orient_matrix_UB_31      0.0514221000
_diffrn_orient_matrix_UB_32      -0.0183756000
_diffrn_orient_matrix_UB_33      -0.0531846000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59742
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.912
_diffrn_reflns_theta_min         3.060
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.158
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62330
_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    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.710
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1504
_refine_ls_number_reflns         20881
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0927P)^2^+10.4070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18098
_reflns_number_total             20881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01416b2.cif
_cod_data_source_block           5
_cod_original_cell_volume        5288.90(13)
_cod_database_code               7702010
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C19H18N4O8CL2ZN1
_reflns_odcompleteness_completeness 99.97
_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, All O(H) groups, All O(H,H) groups
2. Shared sites
{N102, O48}
3. Restrained distances
 H43-O43
 0.9 with sigma of 0.02
 H44B-O44
 0.9 with sigma of 0.02
 O44-H44A
 0.9 with sigma of 0.02
 H41B-O41
 0.9 with sigma of 0.02
 H41A-O41
 0.9 with sigma of 0.02
 H42-O42
 0.9 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl36: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O45) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C113) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(N111) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N105) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N102) = Uanis(O48)
5. Others
 Sof(H77C)=Sof(H77D)=Sof(C78B)=Sof(H78C)=Sof(H78D)=Sof(H79C)=Sof(H79D)=1-FVAR(1)
 Sof(H77A)=Sof(H77B)=Sof(C78A)=Sof(H78A)=Sof(H78B)=Sof(H79A)=Sof(H79B)=FVAR(1)
 Sof(Cl21)=Sof(O22)=Sof(O23)=Sof(O24)=Sof(O25)=1-FVAR(2)
 Sof(Cl26)=Sof(O27)=Sof(O28)=Sof(O29)=Sof(O30)=FVAR(2)
 Sof(Cl37)=Sof(O6)=Sof(O38)=Sof(O40)=1-FVAR(3)
 Sof(Cl36)=Sof(O32)=Sof(O33)=Sof(O34)=FVAR(3)
 Fixed Sof: O45(0.5) O48(0.5) N102(0.5) C103(0.5) C104(0.5) H10C(0.5)
 H10D(0.5) H10E(0.5) O47(0.5) O46(0.5) N96(0.5) C97(0.5) C98(0.5) H98A(0.5)
 H98B(0.5) H98C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,
 H57B), C76(H76A,H76B), C77(H77A,H77B), C77(H77C,H77D), C78A(H78A,H78B),
 C78B(H78C,H78D), C79(H79A,H79B), C79(H79C,H79D), C80(H80A,H80B)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
 C23(H23), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43A), C44(H44),
 C45(H45), C46(H46), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67),
  C68(H68), C69(H69), C83(H83), C84(H84), C85(H85), C86(H86), C89(H89),
 C90(H90), C91(H91), C92(H92)
6.c Idealised Me refined with riding coordinates:
 C98(H98A,H98B,H98C)
6.d Idealised Me refined as rotating group:
 C104(H10C,H10D,H10E), C95(H95A,H95B,H95C), C113(H11C,H11D,H11E), C110(H11F,
 H11G,H11H), C101(H10F,H10G,H10H), C107(H10I,H10J,H10K)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'