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_7702006
_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 H42 N12 Zn, C2 H3 N, C H2 Cl2, 2(Cl O4)'
_chemical_formula_sum            'C75 H47 Cl4 N13 O8 Zn'
_chemical_formula_weight         1465.42
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4058(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.67812(17)
_cell_length_b                   14.09099(13)
_cell_length_c                   26.4871(2)
_cell_measurement_reflns_used    20033
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      73.4840
_cell_measurement_theta_min      3.4050
_cell_volume                     6443.94(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0008451000
_diffrn_orient_matrix_UB_12      0.0075068000
_diffrn_orient_matrix_UB_13      0.0579084000
_diffrn_orient_matrix_UB_21      0.0840682000
_diffrn_orient_matrix_UB_22      0.0366148000
_diffrn_orient_matrix_UB_23      0.0112590000
_diffrn_orient_matrix_UB_31      -0.0298309000
_diffrn_orient_matrix_UB_32      0.1027606000
_diffrn_orient_matrix_UB_33      -0.0081925000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34325
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.997
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.651
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57464
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         12172
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0886P)^2^+14.7646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10438
_reflns_number_total             12172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01416b2.cif
_cod_data_source_block           2
_cod_original_cell_volume        6443.94(11)
_cod_database_code               7702006
_shelxl_version_number           2014-3
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N90) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C93B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3. Same fragment restrains
{C93A, Cl2A, Cl3A}
as
{C93B, Cl2B, Cl3B}
4. Others
 Sof(C93B)=Sof(H93C)=Sof(H93D)=Sof(Cl2B)=Sof(Cl3B)=1-FVAR(1)
 Sof(C93A)=Sof(H93A)=Sof(H93B)=Sof(Cl2A)=Sof(Cl3A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C93A(H93A,H93B), C93B(H93C,H93D)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20),
 C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C36(H36), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49),
 C50(H50), C53(H53), C54(H54), C55(H55), C56(H56), C64(H64), C65(H65), C66(H66),
  C68(H68), C69(H69), C70(H70), C75(H75), C76(H76), C77(H77), C78(H78),
 C81(H81), C82(H82), C83(H83), C84(H84)
5.c Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'