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_7010575
_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
'Pd C18 H18 N2 S2 O 2+, 2(B F4 -), 0.5(C2 H3 N)'
_chemical_formula_sum            'C19 H19.5 B2 F8 N2.5 O Pd S2'
_chemical_formula_weight         643.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.177(4)
_cell_length_b                   11.520(4)
_cell_length_c                   15.006(3)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12.5
_cell_volume                     2266.0(11)
_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  'SHELXTL-97; PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1281
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2128
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 1997b)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.846
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2093
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+57.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1893
_reflns_number_gt                1818
_reflns_number_total             2093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100493j.txt
_cod_data_source_block           Pd(L)(BF4)2.0.5CH3CN
_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_sg_symbol_H-M      C2/m
_cod_original_formula_sum        'C19 H19.50 B2 F8 N2.50 O Pd S2'
_cod_database_code               7010575