Synthesis of a [2]rotaxane incorporating a Ni(II)-salen moiety: evidence of ring-opening-and-closing protocol.
Yoon, Il; Narita, Mamiko; Goto, Midori; Shimizu, Toshimi; Asakawa, Masumi; Organic letters 8 (2006) 2341–2344; doi:10.1021/ol060661m

data_1505992
_publ_section_title
;
 Synthesis of a [2]rotaxane incorporating a Ni(II)-salen moiety: evidence
 of ring-opening-and-closing protocol.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2341
_journal_page_last               2344
_journal_paper_doi               10.1021/ol060661m
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C84.5 H93 Cl3 N3 Ni O24 P2'
_chemical_formula_weight         1761.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.067(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.862(3)
_cell_length_b                   22.782(3)
_cell_length_c                   19.734(3)
_cell_measurement_reflns_used    62314
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      1.03
_cell_volume                     8474(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62314
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.9575
_exptl_absorpt_correction_T_min  0.8441
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.214
_refine_diff_density_min         -2.607
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.91(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2196
_refine_ls_number_reflns         40527
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1934
_refine_ls_R_factor_gt           0.1234
_refine_ls_shift/su_max          1.826
_refine_ls_shift/su_mean         0.092
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1438P)^2^+48.0463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3070
_refine_ls_wR_factor_ref         0.3641
_reflns_number_gt                24656
_reflns_number_total             40527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol060661msi20060322_110000.cif
_cod_data_source_block           rotaxane
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        8475(2)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1505992