Study of temperature and ligand flexibility effects on coordination polymer formation from cyclobutanetetracarboxylic acid
Bello, Lizaira; Quintero, Marilyn; Mora, Asiloé J.; González, Teresa; Escalona, Ana; Añez, Rafael; Ávila, Edward E.; Briceño, Alexander; CrystEngComm 17 (2015) 5921–; doi:10.1039/C5CE00646E

data_7220822
_publ_section_title
;
 Study of temperature and ligand flexibility effects on coordination
 polymer formation from cyclobutanetetracarboxylic acid
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              5921
_journal_paper_doi               10.1039/C5CE00646E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C16 H20 N2 Ni O7, H2 O'
_chemical_formula_sum            'C16 H22 N2 Ni O8'
_chemical_formula_weight         429.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-10-08 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.750(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.956(2)
_cell_length_b                   9.8991(10)
_cell_length_c                   16.960(2)
_cell_measurement_reflns_used    13158
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6002
_cell_measurement_theta_min      1.6702
_cell_volume                     2047.2(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    '<i>DIAMOND</i> Brandenburg (2007)'
_computing_publication_material
'PLATON (Spek, 2003) and publCIF (Westrip, 2010)'
_computing_structure_refinement
'SHELXL-2013 (Sheldrick, 2013), SHELXLE (Hubschle, Sheldrick & Dittrich, 2011)'
_computing_structure_solution
'<i>Superflip</i> (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: 0.0000 - 360.0000
         Image width: 2.0000
            Exp time: 90.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 42.2802
              2theta: -10.0862
scan:
    Number of images: 17
               Slice: -24.0000 - 10.0000
         Image width: 2.0000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 42.2802
              2theta: -10.0862
scan:
    Number of images: 20
               Slice: -30.0000 - 10.0000
         Image width: 2.0000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 42.2802
              2theta: -10.0862
scan:
    Number of images: 20
               Slice: -30.0000 - 10.0000
         Image width: 2.0000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 42.2802
              2theta: -10.0862
scan:
    Number of images: 20
               Slice: -30.0000 - 10.0000
         Image width: 2.0000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 42.2802
              2theta: -10.0862

;
_diffrn_measurement_device_details
;
AFC7: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku, AFC-7 diffractometer'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       'Mercury CCD'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_laue_measured_fraction_full 0.957
_diffrn_reflns_laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23825
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_min         2.057
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998), Private communication'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_recrystallization_method 'Hydrothermal Synthesis'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3874
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0396P)^2^+1.2083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3289
_reflns_number_total             3874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00646e2.cif
_cod_data_source_block           cd09610_001_sq
_cod_depositor_comments
'Adding full bibliography for 7220820--7220822.cif.'
_cod_database_code               7220822
_publcif_datablock.id            {b5506f9b-d370-4c9d-8ca8-84c666f43d8f}
_shelxl_version_number           2013-3
_shelx_res_checksum              16234
_shelx_fab_checksum              57702