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_7219822
_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         'C18 H24 Cu N3 O3 1+, Cl O4 1-, 2(H2 O)'
_chemical_formula_sum            'C18 H28 Cl Cu N3 O9'
_chemical_formula_weight         529.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                nl_kr9
_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                   13.0446(3)
_cell_length_b                   8.8181(2)
_cell_length_c                   19.3686(5)
_cell_measurement_reflns_used    8970
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.758
_cell_measurement_theta_min      3.886
_cell_volume                     2227.94(9)
_computing_cell_refinement       'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_data_collection       'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_data_reduction        'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'enCIFer (CCDC, 2014)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2009)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20122
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.72
_diffrn_reflns_theta_min         2.98
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.7852
_exptl_absorpt_correction_T_min  0.5441
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.36.28.
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_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 Cu(II) perchlorate solution 
at room temperature.
;
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/water'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0638P)^2^+4.0032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                4517
_reflns_number_total             4893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00375j2.cif
_cod_data_source_block           6_Cu-C5
_cod_depositor_comments
'Adding full bibliography for 7219817--7219825.cif.'
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               7219822