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_7219818
_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
'C68 H88 N12 O12 Zn4 4+, 4(Cl O4 1-), 1.5(O H2)'
_chemical_formula_sum            'C68 H91 Cl4 N12 O29.5 Zn4'
_chemical_formula_weight         1951.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                nl_kr12
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5644(3)
_cell_length_b                   34.1856(4)
_cell_length_c                   13.3561(2)
_cell_measurement_reflns_used    25645
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      75.7830
_cell_measurement_theta_min      3.557
_cell_volume                     8019.7(2)
_computing_cell_refinement       'CrysAlisPro (Agilent, V 1.171.37.33)'
_computing_data_collection       'CrysAlisPro (Agilent, V 1.171.37.33)'
_computing_data_reduction        'CrysAlisPro (Agilent, V 1.171.37.33)'
_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(1)
_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_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55998
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         76.63
_diffrn_reflns_theta_min         3.31
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.359
_exptl_absorpt_correction_T_max  0.7749
_exptl_absorpt_correction_T_min  0.5831
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33.
Numerical absorption correction based on gaussian integration over 
a multifaceted crystal model. Empirical absorption correction using 
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4028
_exptl_crystal_preparation
;
Crystals were grown by slow diffusion of a methanolic solution of the 
carboxylic acid ligand into an aqueous Zu(II) perchlorate solution 
at room temperature.
;
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/water'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.217
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         14452
_refine_ls_number_restraints     882
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1020P)^2^+23.5133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                13939
_reflns_number_total             14452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00375j2.cif
_cod_data_source_block           2_Zn-C4
_cod_depositor_comments
'Adding full bibliography for 7219817--7219825.cif.'
_cod_original_sg_symbol_H-M      Pna21
_cod_original_formula_sum        'C68 H91 Cl4 N12 O29.50 Zn4'
_cod_database_code               7219818