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_7702008
_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
'C34 H31 N8 O2 Zn2, 6(Cl0.5 O2), 2.5(H2 O), 0.5(O), 1.5(C H4 O)'
_chemical_formula_sum            'C35.5 H42 Cl3 N8 O18.5 Zn2'
_chemical_formula_weight         1113.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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            8
_cell_length_a                   24.2049(7)
_cell_length_b                   24.8897(8)
_cell_length_c                   14.9855(5)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      2.31
_cell_volume                     9028.1(5)
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            190016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.598
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0835 before and 0.0652 after correction.
The Ratio of minimum to maximum transmission is 0.8695.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         10603
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0554P)^2^+15.5163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7943
_reflns_number_total             10603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01416b2.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C35.50 H42 Cl3 N8 O18.50 Zn2'
_cod_database_code               7702008
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.563
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O52-H52
 0.85 with sigma of 0.02
 O56-H56
 0.85 with sigma of 0.02
 O55-H55A
 0.85 with sigma of 0.02
 O55-H55B
 0.85 with sigma of 0.02
 O54-H54A
 0.85 with sigma of 0.02
 H54-O54
 0.85 with sigma of 0.02
3. Others
 Sof(O16)=Sof(O18)=1-FVAR(1)
 Sof(O17)=Sof(O20)=FVAR(1)
 Fixed Sof: H54A(0.5) H59B(0.5) H53A(0.5) H53B(0.5) H53C(0.5)
4.a Riding coordinates:
 O60(H60A,H60B), O59(H59A,H59B), O57(H57A,H57B)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C25(H25A,H25B), C26(H26A,H26B),
 C36(H36A,H36B), C37(H37A,H37B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20),
 C21(H21), C29(H29), C30(H30), C31(H31), C32(H32), C40(H40), C41(H41), C42(H42),
  C43(H43)
4.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C51(H51A,H51B,H51C)
4.e Idealised tetrahedral OH refined as rotating group:
 O50(H50)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'