Guest-induced stereoselective self-assembly of quinoline-containing Pd(II) and Pt(II) metallacycles
Blanco, Víctor; Abella, Dolores; Rama, Tamara; Alvariño, Cristina; García, Marcos D.; Peinador, Carlos; Quintela, José María; RSC Adv.  (2016) –; doi:10.1039/C6RA14909J

data_7226262
_publ_section_title
;
 Guest-induced stereoselective self-assembly of quinoline-containing
 Pd(II) and Pt(II) metallacycles
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA14909J
_journal_year                    2016
_chemical_formula_sum            'C92 H80 N16 O34 Pd2'
_chemical_formula_weight         2166.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-12 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.801(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.126(5)
_cell_length_b                   20.379(5)
_cell_length_c                   25.002(5)
_cell_measurement_reflns_used    6101
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.101
_cell_measurement_theta_min      5.921
_cell_volume                     9503(4)
_computing_cell_refinement       'SAINT V7.12A (Bruker 2004) in Apex2 suite.'
_computing_data_collection       'Apex2 V.1.0-27 (Bruker, 2005)'
_computing_data_reduction
'SAINT and XPREP 6.14 COPYRIGHT(c) 2003 Bruker-AXS'
_computing_molecular_graphics    'ORTEP3, Chimera 1.10.2'
_computing_publication_material  'ORTEP3, Chimera 1.10.2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Sir92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46176
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_min         1.480
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       prism
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.085
_platon_squeeze_details
;
One of the nitrate counterions in the assymmetric
unit is disordered and could not be modelled adequately
by assigning specific positions to those atoms.
These 8 nitrate anions in the unit cell have been 
treated as a diffuse contribution 
to the overall scattering by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.507
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         11712
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1944P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2475
_refine_ls_wR_factor_ref         0.2962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7215
_reflns_number_total             11712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra14909j2.cif
_cod_data_source_block           shelx
_cod_database_code               7226262
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              56246
_shelx_fab_checksum              94045
_platon_squeeze_void_probe_radius 1.20