#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/25/8102579.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_8102579
loop_
_publ_author_name
'Hai-Xing Liu'
_publ_section_title
;
 Crystal structure of bis(2,9-dimethyl-1,10-phenanthrolinium)
 dichromate dihydrate, [C14H13N2]2[Cr2O7] · 2H2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              717
_journal_volume                  224
_journal_year                    2009
_chemical_formula_sum            'C28 H30 Cr2 N4 O9'
_chemical_formula_weight         670.56
_chemical_name_systematic
; 
Crystal structure of 2,9-dimethyl-1,10-phenanthroline chromate, 
2(C₁₄H₁₂N₂)(Cr₂O₇) 2(H₂O) 2H 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.600(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.268(2)
_cell_length_b                   6.8564(8)
_cell_length_c                   19.9561(18)
_cell_measurement_reflns_used    2067
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.124
_cell_measurement_theta_min      2.172
_cell_volume                     2858.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6805
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.7675
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_meas      1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocky
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0391
_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)+(0.0481P)²+5.5690P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                1765
_reflns_number_total             2489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2797.cff
_cod_data_source_block           090818
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               8102579
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.44385(2) 0.85137(8) 0.65450(3) 0.0350(2) Uani 1 1 d . . .
N1 N 0.23379(11) 0.3545(4) 0.67352(14) 0.0303(6) Uani 1 1 d . . .
H1 H 0.2637 0.3553 0.6624 0.036 Uiso 1 1 calc R . .
N2 N 0.36052(11) 0.3544(4) 0.78588(14) 0.0314(6) Uani 1 1 d . . .
O1 O 0.5000 0.7824(7) 0.7500 0.0854(14) Uani 1 2 d S . .
O2 O 0.39384(11) 0.6744(4) 0.61420(14) 0.0532(7) Uani 1 1 d . . .
O3 O 0.40646(11) 1.0420(4) 0.65553(16) 0.0586(7) Uani 1 1 d . . .
O4 O 0.47952(11) 0.8925(4) 0.60747(14) 0.0574(7) Uani 1 1 d . . .
O5 O 0.68707(12) 0.3570(4) 0.89286(15) 0.0522(7) Uani 1 1 d . . .
C1 C 0.15981(17) 0.3517(6) 0.53341(19) 0.0525(10) Uani 1 1 d . . .
H1A H 0.1996 0.3513 0.5339 0.079 Uiso 0.50 1 calc PR . .
H1B H 0.1356 0.4656 0.5065 0.079 Uiso 0.50 1 calc PR . .
H1C H 0.1358 0.2370 0.5072 0.079 Uiso 0.50 1 calc PR . .
H1D H 0.1144 0.3513 0.4979 0.079 Uiso 0.50 1 calc PR . .
H1E H 0.1784 0.2370 0.5253 0.079 Uiso 0.50 1 calc PR . .
H1F H 0.1782 0.4656 0.5246 0.079 Uiso 0.50 1 calc PR . .
C2 C 0.17301(15) 0.3535(5) 0.61533(18) 0.0365(8) Uani 1 1 d . . .
C3 C 0.12486(14) 0.3548(5) 0.6338(2) 0.0424(9) Uani 1 1 d . . .
H3 H 0.0822 0.3550 0.5939 0.051 Uiso 1 1 calc R . .
C4 C 0.13920(15) 0.3558(5) 0.7092(2) 0.0391(8) Uani 1 1 d . . .
H4 H 0.1064 0.3571 0.7203 0.047 Uiso 1 1 calc R . .
C5 C 0.20313(14) 0.3549(5) 0.77010(18) 0.0334(7) Uani 1 1 d . . .
C6 C 0.25061(14) 0.3545(4) 0.75015(17) 0.0278(7) Uani 1 1 d . . .
C7 C 0.31697(13) 0.3535(4) 0.80932(17) 0.0282(7) Uani 1 1 d . . .
C8 C 0.33315(14) 0.3524(5) 0.88732(17) 0.0337(7) Uani 1 1 d . . .
C9 C 0.39921(16) 0.3475(5) 0.94354(19) 0.0433(8) Uani 1 1 d . . .
H9 H 0.4129 0.3461 0.9964 0.052 Uiso 1 1 calc R . .
C10 C 0.44227(15) 0.3450(5) 0.91944(19) 0.0437(9) Uani 1 1 d . . .
H10 H 0.4858 0.3391 0.9560 0.052 Uiso 1 1 calc R . .
C11 C 0.42189(14) 0.3510(5) 0.83961(19) 0.0349(7) Uani 1 1 d . . .
C12 C 0.46868(15) 0.3523(6) 0.8122(2) 0.0510(10) Uani 1 1 d . . .
H12A H 0.4589 0.2481 0.7757 0.076 Uiso 1 1 calc R . .
H12B H 0.5112 0.3349 0.8558 0.076 Uiso 1 1 calc R . .
H12C H 0.4662 0.4747 0.7874 0.076 Uiso 1 1 calc R . .
C13 C 0.22193(16) 0.3548(5) 0.8507(2) 0.0412(8) Uani 1 1 d . . .
H13 H 0.1906 0.3555 0.8644 0.049 Uiso 1 1 calc R . .
C14 C 0.28400(16) 0.3538(5) 0.90688(19) 0.0406(8) Uani 1 1 d . . .
H14 H 0.2951 0.3540 0.9589 0.049 Uiso 1 1 calc R . .
H5A H 0.6649 0.4583 0.8873 0.060(13) Uiso 1 1 d R . .
H5B H 0.6615 0.2612 0.8770 0.068(14) Uiso 1 1 d R . .
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'
O O 0.0106 0.0060 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Cr1 O3 110.21(14) . . ?
O4 Cr1 O2 109.65(13) . . ?
O3 Cr1 O2 109.50(13) . . ?
O4 Cr1 O1 109.50(10) . . ?
O3 Cr1 O1 109.84(15) . . ?
O2 Cr1 O1 108.10(16) . . ?
C2 N1 C6 122.8(3) . . ?
C2 N1 H1 118.6 . . ?
C6 N1 H1 118.6 . . ?
C11 N2 C7 118.4(3) . . ?
Cr1 O1 Cr1 148.7(3) 2_656 . ?
H5A O5 H5B 106.8 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1A C1 H1D 141.1 . . ?
H1B C1 H1D 56.3 . . ?
H1C C1 H1D 56.3 . . ?
C2 C1 H1E 109.5 . . ?
H1A C1 H1E 56.3 . . ?
H1B C1 H1E 141.1 . . ?
H1C C1 H1E 56.3 . . ?
H1D C1 H1E 109.5 . . ?
C2 C1 H1F 109.5 . . ?
H1A C1 H1F 56.3 . . ?
H1B C1 H1F 56.3 . . ?
H1C C1 H1F 141.1 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?
N1 C2 C3 118.3(3) . . ?
N1 C2 C1 118.5(3) . . ?
C3 C2 C1 123.1(3) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 117.5(3) . . ?
C6 C5 C13 118.9(3) . . ?
C4 C5 C13 123.6(3) . . ?
N1 C6 C5 119.9(3) . . ?
N1 C6 C7 119.5(2) . . ?
C5 C6 C7 120.6(3) . . ?
N2 C7 C8 123.9(3) . . ?
N2 C7 C6 117.5(3) . . ?
C8 C7 C6 118.6(3) . . ?
C7 C8 C9 116.5(3) . . ?
C7 C8 C14 120.2(3) . . ?
C9 C8 C14 123.3(3) . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 120.7(3) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
N2 C11 C10 121.4(3) . . ?
N2 C11 C12 117.2(3) . . ?
C10 C11 C12 121.4(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C5 121.2(3) . . ?
C14 C13 H13 119.4 . . ?
C5 C13 H13 119.4 . . ?
C13 C14 C8 120.5(3) . . ?
C13 C14 H14 119.7 . . ?
C8 C14 H14 119.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 O4 1.593(2) . ?
Cr1 O3 1.597(3) . ?
Cr1 O2 1.612(2) . ?
Cr1 O1 1.7518(13) . ?
N1 C2 1.334(4) . ?
N1 C6 1.367(4) . ?
N1 H1 0.8600 . ?
N2 C11 1.320(4) . ?
N2 C7 1.356(4) . ?
O1 Cr1 1.7518(13) 2_656 ?
O5 H5A 0.8508 . ?
O5 H5B 0.8471 . ?
C1 C2 1.498(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C2 C3 1.392(4) . ?
C3 C4 1.361(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.402(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(4) . ?
C5 C13 1.431(4) . ?
C6 C7 1.432(4) . ?
C7 C8 1.398(4) . ?
C8 C9 1.414(4) . ?
C8 C14 1.432(4) . ?
C9 C10 1.355(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.408(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.490(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.344(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Cr1 O1 Cr1 84.50(12) . . . 2_656 ?
O3 Cr1 O1 Cr1 -36.66(10) . . . 2_656 ?
O2 Cr1 O1 Cr1 -156.08(10) . . . 2_656 ?
C6 N1 C2 C3 0.8(5) . . . . ?
C6 N1 C2 C1 -179.4(3) . . . . ?
N1 C2 C3 C4 -0.5(5) . . . . ?
C1 C2 C3 C4 179.8(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
C3 C4 C5 C13 -179.7(3) . . . . ?
C2 N1 C6 C5 -0.5(5) . . . . ?
C2 N1 C6 C7 179.3(3) . . . . ?
C4 C5 C6 N1 -0.1(5) . . . . ?
C13 C5 C6 N1 180.0(3) . . . . ?
C4 C5 C6 C7 -180.0(3) . . . . ?
C13 C5 C6 C7 0.1(5) . . . . ?
C11 N2 C7 C8 1.0(5) . . . . ?
C11 N2 C7 C6 -179.1(3) . . . . ?
N1 C6 C7 N2 0.5(4) . . . . ?
C5 C6 C7 N2 -179.6(3) . . . . ?
N1 C6 C7 C8 -179.7(3) . . . . ?
C5 C6 C7 C8 0.2(4) . . . . ?
N2 C7 C8 C9 -1.4(5) . . . . ?
C6 C7 C8 C9 178.8(3) . . . . ?
N2 C7 C8 C14 179.3(3) . . . . ?
C6 C7 C8 C14 -0.5(5) . . . . ?
C7 C8 C9 C10 0.2(5) . . . . ?
C14 C8 C9 C10 179.5(3) . . . . ?
C8 C9 C10 C11 1.3(5) . . . . ?
C7 N2 C11 C10 0.5(5) . . . . ?
C7 N2 C11 C12 -179.9(3) . . . . ?
C9 C10 C11 N2 -1.7(5) . . . . ?
C9 C10 C11 C12 178.8(3) . . . . ?
C6 C5 C13 C14 -0.2(5) . . . . ?
C4 C5 C13 C14 179.9(3) . . . . ?
C5 C13 C14 C8 -0.1(5) . . . . ?
C7 C8 C14 C13 0.5(5) . . . . ?
C9 C8 C14 C13 -178.7(3) . . . . ?
