Co-ordination chemistry of 3S-aminopyrrolidine and 3S-(methylamino)pyrrolidine: crystallisation of the two diastereomers of dichloro[3S-(R,S-methylamino)pyrrolidine]palladium(II)
Newman, Paul D.; Hursthouse, Michael B.; Malik, K. M. Abdul; Journal of the Chemical Society, Dalton Transactions  (1999) 599–; doi:10.1039/a808959k

data_7027184
_publ_section_title
;
 Co-ordination chemistry of 3S-aminopyrrolidine and
 3S-(methylamino)pyrrolidine: crystallisation of the two diastereomers of
 dichloro[3S-(R,S-methylamino)pyrrolidine]palladium(II)
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              599
_journal_paper_doi               10.1039/a808959k
_journal_year                    1999
_chemical_formula_moiety         'C5 H12 Cl2 N2 Pd'
_chemical_formula_sum            'C5 H12 Cl2 N2 Pd'
_chemical_formula_weight         277.47
_chemical_name_systematic
;
Dicloro-{3S-(R-methylamino)pyrrolidine}palladium(II)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-96
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2131(4)
_cell_length_b                   10.595(2)
_cell_length_c                   11.664(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      3.32
_cell_volume                     891.4(4)
_computing_cell_refinement       'REFINE in MADNES'
_computing_data_collection       MADNES
_computing_data_reduction        'ABSMAD (Karaulov, 1991)'
_computing_molecular_graphics    'SNOOPI (Davies, 1983)'
_computing_publication_material  SHELXL-96
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'FAST area detector diffractometer'
_diffrn_measurement_method       'Darr, Drake, Hursthouse & Malik, 1993'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4313
_diffrn_reflns_theta_max         29.71
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.612
_exptl_absorpt_correction_T_max  1.106
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   'DIFABS (Walker, 1983)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.898
_refine_ls_goodness_of_fit_obs   0.897
_refine_ls_hydrogen_treatment    'calculated positions, riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_restrained_S_obs      0.897
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_obs          0.0231
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0548
_refine_ls_wR_factor_obs         0.0544
_reflns_number_observed          2183
_reflns_number_total             2203
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808959ksup1.cif
_cod_data_source_block           s92
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        891.4(3)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7027184