Adsorption of water induces a reversible structural phase transition and colour change in new nickel(ii) macrocyclic complexes forming flexible supramolecular networks
Ruiz-Herrera, Brenda Lizette; Flores-Álamo, Marcos; Toscano, Rubén Alfredo; Escudero, Roberto; Sosa-Torres, Martha Elena; New J. Chem. 40 (2016) 7465–; doi:10.1039/C6NJ01621A

data_7055681
_publ_section_title
;
 Adsorption of water induces a reversible structural phase transition and
 colour change in new nickel(ii) macrocyclic complexes forming flexible
 supramolecular networks
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7465
_journal_paper_doi               10.1039/C6NJ01621A
_journal_volume                  40
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C68 H108 Li2 N24 Ni4 O35.5'
_chemical_formula_weight         2078.50
_chemical_name_common            '2- Ni-tpmc-binuclear complex '
_chemical_name_systematic        '[Ni2(tpmc)(?-NO3)](NO3)3 (H2O)2.3H2O'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-06-11 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                87.453(5)
_cell_angle_beta                 89.238(4)
_cell_angle_gamma                83.960(5)
_cell_formula_units_Z            2
_cell_length_a                   11.2964(8)
_cell_length_b                   18.8819(14)
_cell_length_c                   20.7624(13)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.17
_cell_volume                     4399.5(5)
_computing_cell_refinement       'APEX2 v2012.10.0(Bruker, 2012)'
_computing_data_collection       'APEX2 v2012.10.0(Bruker, 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker, 2012)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_publication_material  'CIFTAB V 2013/2 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/1 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2012 (Bruker, 2013)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43154
_diffrn_reflns_point_group_measured_fraction_full 0.725
_diffrn_reflns_point_group_measured_fraction_max 0.692
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.641
_diffrn_reflns_theta_min         1.432
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.944
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_exptl_absorpt_correction_T_min  0.7159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2012)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       prism
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.699
_refine_diff_density_min         -1.992
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 5540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.423(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2524
_refine_ls_number_reflns         28357
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1006P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.412
_reflns_Friedel_fraction_full    0.458
_reflns_Friedel_fraction_max     0.404
_reflns_number_gt                21920
_reflns_number_total             28357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01621a2.cif
_cod_data_source_block           393ATC13
_cod_depositor_comments
'Adding full bibliography for 7055680--7055681.cif.'
_cod_database_code               7055681
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.837
_shelxl_version_number           2014-1
_shelx_res_checksum              55036