One of the most complex small molecule structures ever reported: 16 independent molecules in the asymmetric unit for an ortho-palladated primary amine
Beatrice Braun Irmgard Kalf Ulli Englert; Chem.Commun. 47 (2011) 3846–; doi:10.1039/c0cc05208f

data_7106126
_publ_author_name                'Beatrice Braun Irmgard Kalf Ulli Englert'
_publ_section_title
;
 One of the most complex &#x0093;small molecule structures&#x0094; ever
 reported: 16 independent molecules in the asymmetric unit for an
 ortho-palladated primary amine
;
_journal_name_full               Chem.Commun.
_journal_page_first              3846
_journal_paper_doi               10.1039/c0cc05208f
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C14 H17 Cl N2 O Pd'
_chemical_formula_sum            'C14 H17 Cl N2 O Pd'
_chemical_formula_weight         371.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 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                 109.193(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   19.2521(11)
_cell_length_b                   35.962(2)
_cell_length_c                   18.2585(10)
_cell_measurement_reflns_used    9173
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.93
_cell_measurement_theta_min      2.19
_cell_volume                     11938.5(12)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_sigmaI/netI    0.1095
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            173251
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             5952
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.171
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.29(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2769
_refine_ls_number_reflns         46704
_refine_ls_number_restraints     7237
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                29574
_reflns_number_total             46704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc05208f.txt
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7106126