Spontaneous helical folding of bis(Ni-salphen) complexes in solution and in the solid state: spectroscopic tracking of the unfolding process induced by Na(+) ions.
Achira, Hiroto; Ito, Muneyuki; Mutai, Toshiki; Yoshikawa, Isao; Araki, Koji; Houjou, Hirohiko; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5899–5907; doi:10.1039/c3dt53397b

data_7029451
_publ_section_title
;
 Spontaneous helical folding of bis(Ni-salphen) complexes in solution and
 in the solid state: spectroscopic tracking of the unfolding process
 induced by Na(+) ions.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5899
_journal_page_last               5907
_journal_paper_doi               10.1039/c3dt53397b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C100 H132 N4 Ni2 O8, C2 H6 O'
_chemical_formula_sum            'C102 H138 N4 Ni2 O9'
_chemical_formula_weight         1681.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                64.07(2)
_cell_angle_beta                 79.02(3)
_cell_angle_gamma                72.67(3)
_cell_formula_units_Z            2
_cell_length_a                   13.544(7)
_cell_length_b                   19.397(7)
_cell_length_c                   20.246(10)
_cell_measurement_reflns_used    10704
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.04
_cell_volume                     4555(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'VariMax DW with Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.1568
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30498
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.261
_diffrn_reflns_theta_min         3.040
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         16021
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.0961
_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^)+(0.0814P)^2^+8.3223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9464
_reflns_number_total             16021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53397b2.cif
_cod_data_source_block           shelxl
_cod_database_code               7029451
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.981
_shelxl_version_number           2013-4
_shelx_res_checksum              41988
_shelx_hkl_checksum              31672