Tuning the formation of dicarboxylate linker-assisted supramolecular 1D chains and squares of Ni(ii) using coordination and hydrogen bonds
Khullar, Sadhika; Gupta, Vijay; Mandal, Sanjay K.; CrystEngComm 16 (2014) 5705–; doi:10.1039/c4ce00434e

data_7216124
_publ_section_title
;
 Tuning the formation of dicarboxylate linker-assisted supramolecular 1D
 chains and squares of Ni(ii) using coordination and hydrogen bonds
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              5705
_journal_paper_doi               10.1039/c4ce00434e
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C20 H29 N3 Ni O6, 3(H2 O)'
_chemical_formula_sum            'C20 H35 N3 Ni O9'
_chemical_formula_weight         520.22
_chemical_name_common            '[Ni(bpta)(succinate)(H2O)2].3H2O'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5930(13)
_cell_length_b                   9.6778(7)
_cell_length_c                   17.2357(15)
_cell_measurement_reflns_used    4067
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      23.8232
_cell_measurement_theta_min      2.3633
_cell_volume                     2434.2(4)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo Ka'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16582
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.10
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.307
_refine_ls_abs_structure_details
;
Flack x determined using 1500 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.010(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4267
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0258P)^2^+0.5981P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                3633
_reflns_number_total             4267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00434e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7216121--7216124.cif.'
_cod_database_code               7216124