Metal-mediated formation of liquid crystals: synthesis, structural and thermal analysis of palladium(ii) complexes of crown thioether derivativesElectronic supplementary information (ESI) available: Figs. 1‒3 with full captions, Fig. 4: view of the packing of [Pd(7)][BF4]2. Fig. 5: schematic of undulating layers in [Pd(7)][BF4]2. See http://www.rsc.org/suppdata/cc/b1/b107027b/
Richtzenhain, Heiko; Blake, Alexander J.; Bruce, Duncan W.; Fallis, Ian A.; Li, Wan-Sheung; Schröder, Martin; Chemical Communications  (2001) 2580–; doi:10.1039/b107027b

data_7114837
_publ_section_title
;
 Metal-mediated formation of liquid crystals: synthesis, structural and
 thermal analysis of palladium(ii) complexes of crown thioether
 derivativesElectronic supplementary information (ESI) available: Figs.
 1--3 with full captions, Fig. 4: view of the packing of [Pd(7)][BF4]2.
 Fig. 5: schematic of undulating layers in [Pd(7)][BF4]2. See
 http://www.rsc.org/suppdata/cc/b1/b107027b/
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2580
_journal_paper_doi               10.1039/b107027b
_journal_year                    2001
_chemical_formula_structural     'C28 H36 O6 Pd 2+, 2(BF4) -'
_chemical_formula_sum            'C28 H36 B2 F8 O6 Pd S4'
_chemical_formula_weight         876.83
_chemical_name_common            '[16]aneS4-bisanisate-Pd(II)'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00(5)
_cell_angle_beta                 107.72(3)
_cell_angle_gamma                90.00(5)
_cell_formula_units_Z            2
_cell_length_a                   12.832(5)
_cell_length_b                   10.224(7)
_cell_length_c                   13.609(7)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      10.0
_cell_volume                     1700.7(16)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  'SHELXL93; PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_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  0.043
_diffrn_reflns_av_sigmaI/netI    0.075
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3375
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       tablet
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.09
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2205
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.153
_refine_ls_restrained_S_obs      1.229
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         -0.098
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.034P)^2^+1.044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0922
_refine_ls_wR_factor_obs         0.0797
_reflns_number_observed          1604
_reflns_number_total             2213
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b107027b.txt
_cod_data_source_block           PD16MB
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_geom_bond_publ_flag' value 'Yes' changed to 'yes'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (2
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (2
times).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.034P)^2^+1.044P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.034P)^2^+1.044P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114837