Conformationally locked pentadentate macrocycles containing the 1,10-phenanthroline unit. Synthesis and crystal structure of 5-oxa-2,8-dithia[9](2,9)-1,10-phenanthrolinophane (L) and its coordination properties to NiII, PdII, PtII, RhIII and RuII †
Arca, Massimiliano; Blake, Alexander J.; Casabò, Jaume; Demartin, Francesco; Devillanova, Francesco A.; Garau, Alessandra; Isaia, Francesco; Lippolis, Vito; Kivekas, Raikko; Muns, Vicent; Schröder, Martin; Verani, Gaetano; Journal of the Chemical Society, Dalton Transactions  (2001) 1180–; doi:10.1039/b100493j

data_7010573
_publ_section_title
;
 Conformationally locked pentadentate macrocycles containing the
 1,10-phenanthroline unit. Synthesis and crystal structure of
 5-oxa-2,8-dithia[9](2,9)-1,10-phenanthrolinophane (L) and its
 coordination properties to NiII, PdII, PtII, RhIII and
 RuII&#x200A;&#x2020;
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1180
_journal_paper_doi               10.1039/b100493j
_journal_year                    2001
_chemical_formula_moiety         'C18 H18 N2 O1 S2 0.5(H2 O)'
_chemical_formula_sum            'C18 H19 N2 O1.5 S2'
_chemical_formula_weight         351.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                112.66(3)
_cell_angle_beta                 95.78(4)
_cell_angle_gamma                101.85(2)
_cell_formula_units_Z            4
_cell_length_a                   10.501(2)
_cell_length_b                   13.314(3)
_cell_length_c                   13.579(5)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      14.5
_cell_volume                     1680.3(10)
_computing_cell_refinement       STADI-4
_computing_data_collection       'Stoe STADI-4 (Stoe, 1997a)'
_computing_data_reduction        'Stoe X-RED (Stoe, 1997b)'
_computing_molecular_graphics    'SHELXTL version 5.03 (Siemens, 1994)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       omega/theta
_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  0.00
_diffrn_reflns_av_sigmaI/netI    0.013
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5962
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.60
_refine_diff_density_rms         0.07
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5962
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.250
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+2.0881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                5287
_reflns_number_total             5962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100493j.txt
_cod_data_source_block           L0.5(H2O)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        1680.3(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18 H19 N2 O1.50 S2'
_cod_database_code               7010573