#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/95/4319539.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319539
loop_
_publ_author_name
'Alexander J. Norquist'
'Kevin R. Heier'
'P. Shiv Halasyamani'
'Charlotte L. Stern'
'Kenneth R. Poeppelmeier'
_publ_section_title
;
 Polar Compounds Constructed with the [Cr2O7]2- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2015
_journal_page_last               2019
_journal_paper_doi               10.1021/ic000953y
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'hydro(solvato)thermal synthesis'
_chemical_formula_moiety         'C20 H20 Cr2 Cu N4 O7'
_chemical_formula_sum            'C20 H20 Cr2 Cu N4 O7'
_chemical_formula_weight         595.94
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.927(2)
_cell_length_b                   16.311(2)
_cell_length_c                   8.8513(9)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     2299.4(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution
;
SHELX97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.02332
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21138
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      1.70(5)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       block
_exptl_crystal_F_000             1204.00
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.768
_refine_ls_goodness_of_fit_ref   2.770
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     306
_refine_ls_number_reflns         6213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0340
_refine_ls_wR_factor_ref         0.0340
_reflns_number_gt                6213
_reflns_number_total             7229
_reflns_threshold_expression     I>3.00σ(I)
_cod_data_source_file            ic000953y_1.cif
_cod_data_source_block           '_IC000953Y-Cu(py)4Cr2O7'
_cod_original_cell_volume        2299.4(3)
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C20 H20 Cr2 Cu N4 O7 '
_cod_database_code               4319539
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,1/2+z'
1/2-x,1/2+y,1/2+z
'1/2+x,1/2-y,   +z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Cu(1) 0.20527(1) 0.74747(1) 0.7727 0.01712(5) 1.000 . Uani d ?
Cr(1) 0.19674(2) 0.56571(2) 0.48907(5) 0.02533(8) 1.000 . Uani d ?
Cr(2) 0.29195(2) 0.40279(2) 0.60811(4) 0.02186(8) 1.000 . Uani d ?
O(1) 0.21388(9) 0.64557(8) 0.5944(2) 0.0298(4) 1.000 . Uani d ?
O(2) 0.1011(1) 0.5659(1) 0.4345(2) 0.0611(6) 1.000 . Uani d ?
O(3) 0.2591(1) 0.5638(1) 0.3498(2) 0.0690(7) 1.000 . Uani d ?
O(4) 0.20914(8) 0.47558(8) 0.6036(2) 0.0338(4) 1.000 . Uani d ?
O(5) 0.38181(9) 0.4455(1) 0.6342(2) 0.0404(5) 1.000 . Uani d ?
O(6) 0.29306(9) 0.35040(8) 0.4536(2) 0.0274(4) 1.000 . Uani d ?
O(7) 0.27219(9) 0.34131(9) 0.7466(2) 0.0377(5) 1.000 . Uani d ?
N(1) 0.2946(1) 0.68427(9) 0.8896(2) 0.0193(4) 1.000 . Uani d ?
N(2) 0.1132(1) 0.8083(1) 0.6605(2) 0.0194(4) 1.000 . Uani d ?
N(3) 0.1158(1) 0.68611(9) 0.8904(2) 0.0181(4) 1.000 . Uani d ?
N(4) 0.2911(1) 0.81288(9) 0.6545(2) 0.0175(4) 1.000 . Uani d ?
C(1) 0.2943(1) 0.6004(1) 0.8907(2) 0.0231(5) 1.000 . Uani d ?
C(2) 0.3503(1) 0.5567(1) 0.9767(3) 0.0251(5) 1.000 . Uani d ?
C(3) 0.4091(1) 0.5972(1) 1.0631(2) 0.0334(6) 1.000 . Uani d ?
C(4) 0.4103(1) 0.6819(1) 1.0619(3) 0.0336(6) 1.000 . Uani d ?
C(5) 0.3519(1) 0.7234(1) 0.9728(3) 0.0253(5) 1.000 . Uani d ?
C(6) 0.0559(1) 0.8541(1) 0.7343(2) 0.0249(6) 1.000 . Uani d ?
C(7) -0.0057(1) 0.8974(1) 0.6611(3) 0.0304(6) 1.000 . Uani d ?
C(8) -0.0107(1) 0.8940(1) 0.5068(3) 0.0305(6) 1.000 . Uani d ?
C(9) 0.0490(1) 0.8472(1) 0.4278(3) 0.0300(6) 1.000 . Uani d ?
C(10) 0.1091(1) 0.8052(1) 0.5093(2) 0.0221(5) 1.000 . Uani d ?
C(11) 0.0544(1) 0.6456(1) 0.8163(2) 0.0245(6) 1.000 . Uani d ?
C(12) -0.0087(1) 0.6033(1) 0.8912(2) 0.0257(6) 1.000 . Uani d ?
C(13) -0.0089(1) 0.6022(1) 1.0463(3) 0.0291(6) 1.000 . Uani d ?
C(14) 0.0542(1) 0.6436(1) 1.1247(3) 0.0247(5) 1.000 . Uani d ?
C(15) 0.1151(1) 0.6840(1) 1.0409(2) 0.0218(5) 1.000 . Uani d ?
C(16) 0.2899(1) 0.8947(1) 0.6586(2) 0.0206(5) 1.000 . Uani d ?
C(17) 0.3421(1) 0.9433(1) 0.5713(3) 0.0288(6) 1.000 . Uani d ?
C(18) 0.3983(1) 0.9053(1) 0.4766(3) 0.0336(6) 1.000 . Uani d ?
C(19) 0.4001(1) 0.8210(1) 0.4719(3) 0.0385(7) 1.000 . Uani d ?
C(20) 0.3459(1) 0.7771(1) 0.5604(3) 0.0276(6) 1.000 . Uani d ?
H(1) 0.2535 0.5717 0.8272 0.029 1.000 . Uiso c ?
H(2) 0.3483 0.4975 0.9764 0.029 1.000 . Uiso c ?
H(3) 0.4485 0.5670 1.1229 0.039 1.000 . Uiso c ?
H(4) 0.4500 0.7110 1.1233 0.041 1.000 . Uiso c ?
H(5) 0.3523 0.7826 0.9709 0.031 1.000 . Uiso c ?
H(6) 0.0583 0.8560 0.8434 0.031 1.000 . Uiso c ?
H(7) -0.0453 0.9297 0.7185 0.039 1.000 . Uiso c ?
H(8) -0.0548 0.9228 0.4540 0.036 1.000 . Uiso c ?
H(9) 0.0487 0.8443 0.3188 0.036 1.000 . Uiso c ?
H(10) 0.1506 0.7721 0.4576 0.027 1.000 . Uiso c ?
H(11) 0.0557 0.6468 0.7064 0.030 1.000 . Uiso c ?
H(12) -0.0525 0.5743 0.8356 0.032 1.000 . Uiso c ?
H(13) -0.0524 0.5741 1.1021 0.035 1.000 . Uiso c ?
H(14) 0.0558 0.6438 1.2350 0.031 1.000 . Uiso c ?
H(15) 0.1594 0.7127 1.0946 0.027 1.000 . Uiso c ?
H(16) 0.2512 0.9211 0.7287 0.026 1.000 . Uiso c ?
H(17) 0.3387 1.0027 0.5744 0.037 1.000 . Uiso c ?
H(18) 0.4351 0.9373 0.4125 0.039 1.000 . Uiso c ?
H(19) 0.4389 0.7927 0.4062 0.045 1.000 . Uiso c ?
H(20) 0.3475 0.7182 0.5548 0.032 1.000 . Uiso c ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 80 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
H 0 80 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N 0 16 0.004 0.003
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 28 0.008 0.006
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Cr 0 8 0.284 0.624
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cu 0 4 0.263 1.266
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 CU1 O6 175.92(7) . . . ?
O1 CU1 N1 86.62(9) . . . ?
O1 CU1 N2 93.5(1) . . . ?
O1 CU1 N3 92.17(9) . . . ?
O1 CU1 N4 89.19(9) . . . ?
O6 CU1 N1 90.44(9) 3 3 3 ?
O6 CU1 N2 89.56(9) 3 3 3 ?
O6 CU1 N3 90.60(9) 3 3 3 ?
O6 CU1 N4 88.15(9) 3 3 3 ?
N1 CU1 N2 178.0(1) . . . ?
N1 CU1 N3 88.9(1) . . . ?
N1 CU1 N4 93.30(9) . . . ?
N2 CU1 N3 89.15(9) . . . ?
N2 CU1 N4 88.7(1) . . . ?
N3 CU1 N4 177.5(1) . . . ?
O1 CR1 O2 109.4(2) . . . ?
O1 CR1 O3 110.9(1) . . . ?
O1 CR1 O4 108.3(1) . . . ?
O2 CR1 O3 111.3(2) . . . ?
O2 CR1 O4 106.1(1) . . . ?
O3 CR1 O4 110.8(1) . . . ?
O4 CR2 O5 112.0(1) . . . ?
O4 CR2 O6 110.1(1) . . . ?
O4 CR2 O7 106.7(1) . . . ?
O5 CR2 O6 110.0(1) . . . ?
O5 CR2 O7 109.5(1) . . . ?
O6 CR2 O7 108.5(1) . . . ?
CU1 O1 CR1 164.7(1) . . . ?
CU1 O6 CR2 165.7(1) 3_544 3_544 3_544 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
CU1 O1 2.296(2) . . ?
CU1 O6 2.320(2) . . ?
CU1 N1 2.039(3) . . ?
CU1 N2 2.030(3) . . ?
CU1 N3 2.029(2) . . ?
CU1 N4 2.025(2) . . ?
CR1 O1 1.625(2) . . ?
CR1 O2 1.598(3) . . ?
CR1 O3 1.584(3) . . ?
CR1 O4 1.797(2) . . ?
CR2 O4 1.775(2) . . ?
CR2 O5 1.608(2) . . ?
CR2 O6 1.612(2) . . ?
CR2 O7 1.615(2) . . ?
