Versatile coordination behaviour of an asymmetric half-salen ligand bearing a dansyl fluorophore.
Romero, María J; Pedrido, Rosa; González-Noya, Ana M; Maneiro, Marcelino; Fernández-García, M Isabel; Zaragoza, Guillermo; Bermejo, Manuel R.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 10832–10844; doi:10.1039/c2dt31093g

data_7020028
_publ_section_title
;
 Versatile coordination behaviour of an asymmetric half-salen ligand
 bearing a dansyl fluorophore.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10832
_journal_page_last               10844
_journal_paper_doi               10.1039/c2dt31093g
_journal_volume                  41
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H27 N3 Ni O6 S, C4 H10 O, H2 O'
_chemical_formula_sum            'C29 H39 N3 Ni O8 S'
_chemical_formula_weight         648.4
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-03-01T12:55:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                67.060(14)
_cell_angle_beta                 80.500(10)
_cell_angle_gamma                77.410(8)
_cell_formula_units_Z            2
_cell_length_a                   11.3061(11)
_cell_length_b                   11.4223(19)
_cell_length_c                   12.998(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.14
_cell_measurement_theta_min      12.83
_cell_measurement_wavelength     1.54184
_cell_volume                     1502.7(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.010432
_diffrn_orient_matrix_UB_12      0.016494
_diffrn_orient_matrix_UB_13      -0.082110
_diffrn_orient_matrix_UB_21      -0.031587
_diffrn_orient_matrix_UB_22      0.093776
_diffrn_orient_matrix_UB_23      -0.016586
_diffrn_orient_matrix_UB_31      0.084693
_diffrn_orient_matrix_UB_32      0.015424
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Cuk\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6363
_diffrn_reflns_theta_full        73.42
_diffrn_reflns_theta_max         73.42
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.038
_exptl_absorpt_correction_T_max  0.8850
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 7
Theta correction was applied.
Weighted transmission curves were used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6038
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+0.3017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                4945
_reflns_number_total             6038
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2dt31093g.txt
_cod_data_source_block           NiOH
_cod_database_code               7020028
_exptl_absorpt_factor_mur        0.107
_exptl_absorpt_correction_t_ave  0.8104
_exptl_absorpt_rmerge_before     0.0421
_exptl_absorpt_rmerge_after      0.0421
_exptl_absorpt_theta_corr_max    1.0000
_exptl_absorpt_theta_corr_min    0.9967
_diffrn_standards_decay_corr_max 1.061
_diffrn_standards_decay_corr_min 0.979