Alkyl linker effects on the coordination topology of ditopic di(2-pyridylmethyl)amine carboxylate ligands with ZnIIand CuII: polymers vs. macrocycles
Rodpun, Kiattipoom; Blackman, Allan G.; Gardiner, Michael G.; Tan, Eng Wui; Meledandri, Carla J.; Lucas, Nigel T.; CrystEngComm 17 (2015) 2974–; doi:10.1039/C5CE00375J

data_7219825
_publ_section_title
;
 Alkyl linker effects on the coordination topology of ditopic
 di(2-pyridylmethyl)amine carboxylate ligands with ZnIIand CuII: polymers
 vs. macrocycles
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2974
_journal_paper_doi               10.1039/C5CE00375J
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'C48 H72 N6 O6 Zn2 2+, C48 H68 N6 O4 Zn2 2+, 4(Cl O4 1-), H2 O'
_chemical_formula_sum            'C96 H142 Cl4 N12 O27 Zn4'
_chemical_formula_weight         2299.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                30krzn
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-22 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   36.788(7)
_cell_length_b                   8.6690(17)
_cell_length_c                   33.481(7)
_cell_measurement_reflns_used    22129
_cell_measurement_temperature    100(2)
_cell_volume                     10433(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'BLU-ICE (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'enCIFer (CCDC, 2014)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment
; 
Crystal was attached to a CryoLoop supported in a copper mounting pin, 
then quenched in a cold nitrogen gas at 100 K.
;
_diffrn_detector_area_resol_mean 'ADSC Q315'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  '3-ID1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_source         'Synchrotron ID'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            81232
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.17
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4824
_exptl_crystal_preparation
;
Crystals were grown by slow diffusion of a methanolic solution of the 
carboxylic acid ligand into an aqueous Zn(II) perchlorate solution 
at room temperature.
;
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/water'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1304
_refine_ls_number_reflns         17724
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+21.9822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                17224
_reflns_number_total             17724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00375j2.cif
_cod_data_source_block           9_Zn-C11
_cod_depositor_comments
'Adding full bibliography for 7219817--7219825.cif.'
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7219825