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_7219817
_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         'C16 H20 N3 O3 Zn 1+, Cl O4 1-, 3.5(H2 O)'
_chemical_formula_sum            'C16 H27 Cl N3 O10.5 Zn'
_chemical_formula_weight         530.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                nl_kr3
_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                 104.058(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0642(10)
_cell_length_b                   19.594(2)
_cell_length_c                   12.6956(15)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      30.3364
_cell_measurement_theta_min      2.4979
_cell_volume                     2187.3(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_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      92(2)
_diffrn_crystal_treatment
; 
Crystal was attached with Paratone N oil to a 0.3 mm CryoLoop supported 
in a copper mounting pin, then quenched in a cold nitrogen gas from a gas
stream from an Oxford Cryosystems Cryostream.
;
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa X8 ApexII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38578
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_T_max  0.9258
_exptl_absorpt_correction_T_min  0.5974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1100
_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          0.44
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6661
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+11.2612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                5578
_reflns_number_total             6661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00375j2.cif
_cod_data_source_block           1_Zn-C3
_cod_depositor_comments
'Adding full bibliography for 7219817--7219825.cif.'
_cod_original_cell_volume        2187.2(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C16 H27 Cl N3 O10.50 Zn'
_cod_database_code               7219817