A hydroquinone based palladium catalyst for room temperature nitro reduction in water
Kumar, Alok; Purkait, Kallol; Dey, Suman Kr.; Sarkar, Amrita; Mukherjee, Arindam; RSC Advances 4 (2014) 35233–; doi:10.1039/C4RA06547F

data_7217734
_publ_section_title
;
 A hydroquinone based palladium catalyst for room temperature nitro
 reduction in water
;
_journal_issue                   66
_journal_name_full               'RSC Advances'
_journal_page_first              35233
_journal_paper_doi               10.1039/C4RA06547F
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C16 H18 Cl2 N4 O2 Pd, 2(O)'
_chemical_formula_sum            'C16 H22 Cl2 N4 O4 Pd'
_chemical_formula_weight         511.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3889(10)
_cell_length_b                   8.8163(3)
_cell_length_c                   14.1318(4)
_cell_measurement_reflns_used    1186
_cell_measurement_temperature    100(2)
_cell_volume                     2041.90(15)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2816
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1921
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                1805
_reflns_number_total             1921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra06547f2.cif
_cod_data_source_block           ak1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               7217734
_check_cif_alert_explanations
;
PLAT306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) .......        O1S
Comment: O1S is a solvent water molecule in the lattice for which the H atoms
could not be located.
;