#------------------------------------------------------------------------------
#$Date: 2017-10-13 09:09:21 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/23/2202331.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2202331
loop_
_publ_author_name
'Srinivasan, Bikshandarkoil R. '
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 Piperazinium chromate(VI)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m639
_journal_page_last               m641
_journal_paper_doi               10.1107/S1600536803014879
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C4 H12 N2 2+, O4 Cr 2-'
_chemical_formula_moiety         'C4 H12 N2 2+, O4 Cr 2-'
_chemical_formula_sum            'C4 H12 Cr N2 O4'
_chemical_formula_weight         204.16
_chemical_name_common            'Piperazinium chromate(VI)'
_chemical_name_systematic
;
Piperazinium chromate(VI)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.766(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6651(9)
_cell_length_b                   12.3726(18)
_cell_length_c                   8.4886(10)
_cell_measurement_reflns_used    105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      16
_cell_volume                     803.30(18)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1998)'
_computing_publication_material  'CIFTAB in SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe AED-II four-circle'
_diffrn_measurement_method       ω
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4578
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED; Stoe & Cie, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.523
_refine_ls_extinction_coef       0.105(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0263
_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/[σ²(Fo²)+(0.0429P)²+0.3211P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                2034
_reflns_number_total             2350
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6299.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2202331
_cod_database_fobs_code          2202331
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cr1 0.21819(3) 0.910006(19) 0.17835(3) 0.02268(10) Uani d . 1 . . Cr
O1 0.03085(15) 0.90257(10) 0.26610(15) 0.0314(2) Uani d . 1 . . O
O2 0.20805(17) 0.81921(11) 0.03380(13) 0.0346(3) Uani d . 1 . . O
O3 0.38107(15) 0.88111(13) 0.30737(14) 0.0392(3) Uani d . 1 . . O
O4 0.2389(2) 1.02997(12) 0.10613(18) 0.0495(4) Uani d . 1 . . O
N1 0.14987(18) 0.91284(11) 0.74774(15) 0.0270(3) Uani d . 1 . . N
H1N1 0.0788 0.9706 0.7508 0.032 Uiso calc R 1 . . H
H2N1 0.1610 0.8842 0.8453 0.032 Uiso calc R 1 . . H
C1 0.0691(2) 0.83133(14) 0.63617(18) 0.0291(3) Uani d . 1 . . C
H1A 0.0490 0.8631 0.5321 0.035 Uiso calc R 1 . . H
H1B -0.0426 0.8083 0.6719 0.035 Uiso calc R 1 . . H
C2 0.1892(2) 0.73577(14) 0.6280(2) 0.0328(3) Uani d . 1 . . C
H2A 0.2012 0.7006 0.7303 0.039 Uiso calc R 1 . . H
H2B 0.1395 0.6841 0.5518 0.039 Uiso calc R 1 . . H
N2 0.36406(18) 0.77052(13) 0.58131(16) 0.0330(3) Uani d . 1 . . N
H1N2 0.3535 0.7987 0.4834 0.040 Uiso calc R 1 . . H
H2N2 0.4349 0.7126 0.5793 0.040 Uiso calc R 1 . . H
C3 0.4435(2) 0.85223(15) 0.6925(2) 0.0343(3) Uani d . 1 . . C
H3A 0.5551 0.8755 0.6569 0.041 Uiso calc R 1 . . H
H3B 0.4638 0.8204 0.7966 0.041 Uiso calc R 1 . . H
C4 0.3232(2) 0.94819(14) 0.7014(2) 0.0334(3) Uani d . 1 . . C
H4A 0.3729 0.9997 0.7780 0.040 Uiso calc R 1 . . H
H4B 0.3110 0.9837 0.5994 0.040 Uiso calc R 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cr1 0.02214(14) 0.02577(14) 0.01977(13) -0.00299(8) -0.00120(8) 0.00162(8)
O1 0.0264(5) 0.0316(6) 0.0369(6) 0.0027(4) 0.0064(4) -0.0005(5)
O2 0.0438(7) 0.0370(7) 0.0232(5) -0.0006(5) 0.0033(5) -0.0036(4)
O3 0.0258(5) 0.0605(9) 0.0304(6) -0.0027(5) -0.0055(4) 0.0051(6)
O4 0.0655(9) 0.0360(7) 0.0462(7) -0.0165(7) -0.0024(7) 0.0122(6)
N1 0.0289(6) 0.0278(6) 0.0245(6) 0.0051(5) 0.0034(5) -0.0006(5)
C1 0.0250(6) 0.0326(8) 0.0294(7) -0.0016(6) -0.0019(5) 0.0018(6)
C2 0.0413(8) 0.0237(7) 0.0324(7) -0.0016(6) -0.0048(6) -0.0023(6)
N2 0.0330(6) 0.0370(7) 0.0285(6) 0.0144(6) -0.0009(5) -0.0042(6)
C3 0.0233(7) 0.0395(9) 0.0395(8) 0.0018(6) -0.0017(6) -0.0024(7)
C4 0.0314(7) 0.0257(7) 0.0432(9) -0.0036(6) 0.0031(6) -0.0020(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O4 Cr1 O3 111.27(8) y
O4 Cr1 O2 109.97(7) y
O3 Cr1 O2 109.96(7) y
O4 Cr1 O1 109.23(8) y
O3 Cr1 O1 109.25(6) y
O2 Cr1 O1 107.07(6) y
C4 N1 C1 112.01(12) y
C4 N1 H1N1 109.2 n
C1 N1 H1N1 109.2 n
C4 N1 H2N1 109.2 n
C1 N1 H2N1 109.2 n
H1N1 N1 H2N1 107.9 n
N1 C1 C2 109.36(13) y
N1 C1 H1A 109.8 n
C2 C1 H1A 109.8 n
N1 C1 H1B 109.8 n
C2 C1 H1B 109.8 n
H1A C1 H1B 108.3 n
N2 C2 C1 110.52(14) y
N2 C2 H2A 109.5 n
C1 C2 H2A 109.5 n
N2 C2 H2B 109.5 n
C1 C2 H2B 109.5 n
H2A C2 H2B 108.1 n
C2 N2 C3 111.48(12) y
C2 N2 H1N2 109.3 n
C3 N2 H1N2 109.3 n
C2 N2 H2N2 109.3 n
C3 N2 H2N2 109.3 n
H1N2 N2 H2N2 108.0 n
N2 C3 C4 109.94(13) y
N2 C3 H3A 109.7 n
C4 C3 H3A 109.7 n
N2 C3 H3B 109.7 n
C4 C3 H3B 109.7 n
H3A C3 H3B 108.2 n
N1 C4 C3 110.10(14) y
N1 C4 H4A 109.6 n
C3 C4 H4A 109.6 n
N1 C4 H4B 109.6 n
C3 C4 H4B 109.6 n
H4A C4 H4B 108.2 n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cr1 O4 . 1.6176(14) y
Cr1 O3 . 1.6451(12) y
Cr1 O2 . 1.6617(12) y
Cr1 O1 . 1.6631(12) y
N1 C4 . 1.476(2) y
N1 C1 . 1.490(2) y
N1 H1N1 . 0.9000 n
N1 H2N1 . 0.9000 n
C1 C2 . 1.503(2) y
C1 H1A . 0.9700 n
C1 H1B . 0.9700 n
C2 N2 . 1.486(2) y
C2 H2A . 0.9700 n
C2 H2B . 0.9700 n
N2 C3 . 1.486(2) y
N2 H1N2 . 0.9000 n
N2 H2N2 . 0.9000 n
C3 C4 . 1.508(2) y
C3 H3A . 0.9700 n
C3 H3B . 0.9700 n
C4 H4A . 0.9700 n
C4 H4B . 0.9700 n
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1N1 O1 3_576 0.90 1.78 2.6697(18) 169
N1 H2N1 O2 1_556 0.90 1.81 2.7009(18) 173
N2 H1N2 O3 . 0.90 1.83 2.709(2) 164
N2 H2N2 O2 4_676 0.90 2.19 2.9133(19) 137
N2 H2N2 O1 4_676 0.90 2.22 2.9014(19) 132
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30654702
