Expanding the Cavity Size: Preparation of 2:1 Inclusion Complexes Based on Dinuclear Square Metallocycles
Víctor Blanco; Albert Gutiérrez; Carlos Platas-Iglesias; Carlos Peinador; José M. Quintela; Journal of Organic Chemistry 74 (2009) 6577–6583; doi:10.1021/jo901034c

data_4024799
_publ_section_title
;
Expanding the Cavity Size: Preparation of 2:1 Inclusion Complexes Based on
Dinuclear Square Metallocycles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6577
_journal_page_last               6583
_journal_paper_doi               10.1021/jo901034c
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C93 H96 F45 N21 O24 P4.5 Pd3 S6'
_chemical_formula_weight         3382.36
_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                 111.639(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.957(2)
_cell_length_b                   19.8218(14)
_cell_length_c                   36.046(4)
_cell_measurement_reflns_used    9277
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.401
_cell_measurement_theta_min      5.038
_cell_volume                     18567(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1089
_diffrn_reflns_av_sigmaI/netI    0.1021
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            69150
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         0.61
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.8404
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6690
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.225
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.512
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         16981
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.511
_refine_ls_R_factor_all          0.2306
_refine_ls_R_factor_gt           0.1481
_refine_ls_shift/su_max          0.170
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4005
_refine_ls_wR_factor_ref         0.4487
_reflns_number_gt                9198
_reflns_number_total             16981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901034c_si_002.cif
_cod_data_source_block           0732803_1s
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_original_formula_sum        'C93 H96 F45 N21 O24 P4.50 Pd3 S6'
_cod_database_code               4024799