#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/30/2223036.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_2223036
loop_
_publ_author_name
'Liu, Hai-Xing'
'Dong, Gui-Ying'
'Ma, Zhi-Hong'
'Cui, Guang-Hua'
_publ_section_title
;
 Diaquabis(1,10-phenanthroline)magnesium dichromate(VI)
 1,10-phenanthroline disolvate
;
_journal_coeditor_code           CV2597
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1026
_journal_paper_doi               10.1107/S1600536809030128
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Mg (C12 H8 N2)2 (H2 O)2] [Cr2 O7], 2C12 H8 N2'
_chemical_formula_moiety
'C24 H20 Mg N4 O2 2+, Cr2 O7 2-, 2(C12 H8 N2)'
_chemical_formula_sum            'C48 H36 Cr2 Mg N8 O9'
_chemical_formula_weight         997.16
_chemical_name_systematic
;Diaquabis(1,10-phenanthroline)magnesium(II) dichromate(VI)
 1,10-phenanthroline
disolvate
;
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 123.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.761(3)
_cell_length_b                   22.172(4)
_cell_length_c                   13.996(3)
_cell_measurement_reflns_used    2800
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.81
_cell_measurement_theta_min      5.02
_cell_volume                     4338(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16762
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0507
_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/[σ²(Fo²)+(0.0878P)²+5.6611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                3068
_reflns_number_total             3817
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2597.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C48 H36 Cr2 Mg N8 O9 '
_cod_database_code               2223036
_cod_database_fobs_code          2223036
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_type_symbol
_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
O O4 0.5000 0.0547(2) 0.2500 0.135(2) Uani d S 1 . .
Mg Mg1 0.5000 0.32609(6) 0.2500 0.0429(3) Uani d S 1 . .
C C12 0.42272(18) 0.41277(11) 0.3486(2) 0.0341(6) Uani d . 1 . .
C C4 0.36810(18) 0.45551(13) 0.3620(2) 0.0387(6) Uani d . 1 . .
N N1 0.40575(15) 0.39775(10) 0.24512(19) 0.0374(5) Uani d . 1 . .
N N2 0.55208(16) 0.34161(11) 0.4315(2) 0.0427(6) Uani d . 1 . .
C C7 0.5222(2) 0.39865(14) 0.5573(2) 0.0431(7) Uani d . 1 . .
C C11 0.50124(18) 0.38299(12) 0.4484(2) 0.0367(6) Uani d . 1 . .
O O1W 0.60296(19) 0.26585(11) 0.2850(2) 0.0743(8) Uani d . 1 . .
C C5 0.3893(2) 0.46843(14) 0.4739(3) 0.0479(7) Uani d . 1 . .
H H5 0.3515 0.4957 0.4826 0.057 Uiso calc R 1 . .
C C2 0.2783(2) 0.46981(15) 0.1593(3) 0.0503(7) Uani d . 1 . .
H H2 0.2303 0.4890 0.0930 0.060 Uiso calc R 1 . .
C C3 0.2941(2) 0.48458(14) 0.2624(3) 0.0471(7) Uani d . 1 . .
H H3 0.2565 0.5136 0.2674 0.057 Uiso calc R 1 . .
C C6 0.4639(2) 0.44126(15) 0.5673(3) 0.0509(8) Uani d . 1 . .
H H6 0.4772 0.4507 0.6395 0.061 Uiso calc R 1 . .
C C10 0.6264(2) 0.31578(16) 0.5247(3) 0.0557(8) Uani d . 1 . .
H H10 0.6616 0.2871 0.5145 0.067 Uiso calc R 1 . .
C C1 0.3345(2) 0.42583(14) 0.1536(3) 0.0469(7) Uani d . 1 . .
H H1 0.3217 0.4155 0.0820 0.056 Uiso calc R 1 . .
C C9 0.6539(2) 0.32924(18) 0.6350(3) 0.0637(10) Uani d . 1 . .
H H9 0.7068 0.3104 0.6971 0.076 Uiso calc R 1 . .
C C8 0.6026(2) 0.37051(17) 0.6519(3) 0.0575(9) Uani d . 1 . .
H H8 0.6205 0.3801 0.7260 0.069 Uiso calc R 1 . .
H H1B 0.5962 0.2278 0.2851 0.086 Uiso d R 1 . .
H H1A 0.6369 0.2686 0.2572 0.086 Uiso d R 1 . .
C C24 0.7163(2) 0.30719(14) 0.1147(3) 0.0448(7) Uani d . 1 . .
C C16 0.7005(2) 0.32042(15) 0.0067(3) 0.0496(7) Uani d . 1 . .
C C23 0.7918(2) 0.33854(14) 0.2156(3) 0.0467(7) Uani d . 1 . .
C C19 0.8456(2) 0.38268(16) 0.2027(3) 0.0513(8) Uani d . 1 . .
N N3 0.66308(19) 0.26634(13) 0.1282(2) 0.0533(7) Uani d . 1 . .
N N4 0.8060(2) 0.32422(14) 0.3182(2) 0.0577(7) Uani d . 1 . .
C C18 0.8266(2) 0.39479(17) 0.0912(3) 0.0585(9) Uani d . 1 . .
H H18 0.8621 0.4241 0.0830 0.070 Uiso calc R 1 . .
C C17 0.7583(2) 0.36451(18) -0.0013(3) 0.0590(9) Uani d . 1 . .
H H17 0.7486 0.3725 -0.0722 0.071 Uiso calc R 1 . .
C C13 0.5949(3) 0.23787(17) 0.0359(3) 0.0611(9) Uani d . 1 . .
H H13 0.5584 0.2097 0.0448 0.073 Uiso calc R 1 . .
C C14 0.5743(3) 0.24734(17) -0.0736(3) 0.0641(9) Uani d . 1 . .
H H14 0.5252 0.2262 -0.1358 0.077 Uiso calc R 1 . .
C C20 0.9162(2) 0.41347(18) 0.3012(3) 0.0642(10) Uani d . 1 . .
H H20 0.9527 0.4434 0.2963 0.077 Uiso calc R 1 . .
C C15 0.6273(2) 0.28822(17) -0.0877(3) 0.0601(9) Uani d . 1 . .
H H15 0.6151 0.2949 -0.1602 0.072 Uiso calc R 1 . .
C C21 0.9307(3) 0.3991(2) 0.4040(3) 0.0712(11) Uani d . 1 . .
H H21 0.9775 0.4188 0.4704 0.085 Uiso calc R 1 . .
C C22 0.8749(3) 0.35454(19) 0.4088(3) 0.0681(10) Uani d . 1 . .
H H22 0.8863 0.3452 0.4801 0.082 Uiso calc R 1 . .
Cr Cr1 0.60986(4) 0.08803(3) 0.29232(5) 0.0543(2) Uani d . 1 . .
O O2 0.69117(19) 0.04355(13) 0.3843(2) 0.0739(8) Uani d . 1 . .
O O3 0.6203(3) 0.09376(18) 0.1873(2) 0.1033(11) Uani d . 1 . .
O O1 0.6225(2) 0.15268(13) 0.3521(3) 0.0874(9) Uani d . 1 . .
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'
Mg Mg 0.0486 0.0363 '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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cr1 O4 Cr1 . 2_655 130.3(3) ?
O1W Mg1 O1W 2_655 . 97.08(17) ?
O1W Mg1 N2 2_655 . 97.14(10) ?
O1W Mg1 N2 . . 94.70(11) ?
O1W Mg1 N2 2_655 2_655 94.70(11) ?
O1W Mg1 N2 . 2_655 97.14(10) ?
N2 Mg1 N2 . 2_655 162.09(14) ?
O1W Mg1 N1 2_655 . 88.13(10) ?
O1W Mg1 N1 . . 169.28(11) ?
N2 Mg1 N1 . . 75.31(9) ?
N2 Mg1 N1 2_655 . 91.73(9) ?
O1W Mg1 N1 2_655 2_655 169.28(10) ?
O1W Mg1 N1 . 2_655 88.13(10) ?
N2 Mg1 N1 . 2_655 91.73(9) ?
N2 Mg1 N1 2_655 2_655 75.31(9) ?
N1 Mg1 N1 . 2_655 88.32(13) ?
N1 C12 C4 . . 122.9(2) ?
N1 C12 C11 . . 117.6(2) ?
C4 C12 C11 . . 119.5(2) ?
C12 C4 C3 . . 117.3(3) ?
C12 C4 C5 . . 119.8(3) ?
C3 C4 C5 . . 122.9(3) ?
C1 N1 C12 . . 117.6(2) ?
C1 N1 Mg1 . . 127.7(2) ?
C12 N1 Mg1 . . 114.72(17) ?
C10 N2 C11 . . 117.1(3) ?
C10 N2 Mg1 . . 128.2(2) ?
C11 N2 Mg1 . . 114.65(18) ?
C11 C7 C8 . . 116.6(3) ?
C11 C7 C6 . . 119.8(3) ?
C8 C7 C6 . . 123.7(3) ?
N2 C11 C7 . . 123.3(2) ?
N2 C11 C12 . . 117.7(2) ?
C7 C11 C12 . . 119.0(3) ?
Mg1 O1W H1B . . 124.0 ?
Mg1 O1W H1A . . 122.7 ?
H1B O1W H1A . . 101.3 ?
C6 C5 C4 . . 120.5(3) ?
C6 C5 H5 . . 119.8 ?
C4 C5 H5 . . 119.8 ?
C3 C2 C1 . . 119.4(3) ?
C3 C2 H2 . . 120.3 ?
C1 C2 H2 . . 120.3 ?
C2 C3 C4 . . 119.4(3) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C5 C6 C7 . . 121.4(3) ?
C5 C6 H6 . . 119.3 ?
C7 C6 H6 . . 119.3 ?
N2 C10 C9 . . 123.7(3) ?
N2 C10 H10 . . 118.1 ?
C9 C10 H10 . . 118.1 ?
N1 C1 C2 . . 123.4(3) ?
N1 C1 H1 . . 118.3 ?
C2 C1 H1 . . 118.3 ?
C8 C9 C10 . . 119.2(3) ?
C8 C9 H9 . . 120.4 ?
C10 C9 H9 . . 120.4 ?
C9 C8 C7 . . 120.1(3) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
N3 C24 C16 . . 122.5(3) ?
N3 C24 C23 . . 118.2(3) ?
C16 C24 C23 . . 119.3(3) ?
C15 C16 C24 . . 116.8(3) ?
C15 C16 C17 . . 123.7(3) ?
C24 C16 C17 . . 119.5(3) ?
N4 C23 C19 . . 123.2(3) ?
N4 C23 C24 . . 117.8(3) ?
C19 C23 C24 . . 119.0(3) ?
C20 C19 C23 . . 117.7(3) ?
C20 C19 C18 . . 122.6(3) ?
C23 C19 C18 . . 119.7(3) ?
C13 N3 C24 . . 117.6(3) ?
C22 N4 C23 . . 116.3(3) ?
C17 C18 C19 . . 121.0(3) ?
C17 C18 H18 . . 119.5 ?
C19 C18 H18 . . 119.5 ?
C18 C17 C16 . . 121.4(3) ?
C18 C17 H17 . . 119.3 ?
C16 C17 H17 . . 119.3 ?
N3 C13 C14 . . 124.2(3) ?
N3 C13 H13 . . 117.9 ?
C14 C13 H13 . . 117.9 ?
C15 C14 C13 . . 118.5(3) ?
C15 C14 H14 . . 120.7 ?
C13 C14 H14 . . 120.7 ?
C21 C20 C19 . . 119.2(4) ?
C21 C20 H20 . . 120.4 ?
C19 C20 H20 . . 120.4 ?
C14 C15 C16 . . 120.3(3) ?
C14 C15 H15 . . 119.9 ?
C16 C15 H15 . . 119.9 ?
C20 C21 C22 . . 119.2(4) ?
C20 C21 H21 . . 120.4 ?
C22 C21 H21 . . 120.4 ?
N4 C22 C21 . . 124.4(4) ?
N4 C22 H22 . . 117.8 ?
C21 C22 H22 . . 117.8 ?
O3 Cr1 O2 . . 108.43(17) ?
O3 Cr1 O1 . . 111.17(19) ?
O2 Cr1 O1 . . 108.75(16) ?
O3 Cr1 O4 . . 110.76(14) ?
O2 Cr1 O4 . . 106.38(17) ?
O1 Cr1 O4 . . 111.18(18) ?
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
O4 Cr1 . 1.756(2) ?
O4 Cr1 2_655 1.756(2) ?
Mg1 O1W 2_655 2.017(2) ?
Mg1 O1W . 2.017(2) ?
Mg1 N2 . 2.210(3) ?
Mg1 N2 2_655 2.210(3) ?
Mg1 N1 . 2.215(2) ?
Mg1 N1 2_655 2.215(2) ?
C12 N1 . 1.354(3) ?
C12 C4 . 1.401(4) ?
C12 C11 . 1.446(4) ?
C4 C3 . 1.410(4) ?
C4 C5 . 1.431(4) ?
N1 C1 . 1.329(4) ?
N2 C10 . 1.337(4) ?
N2 C11 . 1.359(4) ?
C7 C11 . 1.406(4) ?
C7 C8 . 1.410(4) ?
C7 C6 . 1.421(5) ?
O1W H1B . 0.8517 ?
O1W H1A . 0.8491 ?
C5 C6 . 1.353(5) ?
C5 H5 . 0.9300 ?
C2 C3 . 1.356(5) ?
C2 C1 . 1.389(4) ?
C2 H2 . 0.9300 ?
C3 H3 . 0.9300 ?
C6 H6 . 0.9300 ?
C10 C9 . 1.378(5) ?
C10 H10 . 0.9300 ?
C1 H1 . 0.9300 ?
C9 C8 . 1.363(5) ?
C9 H9 . 0.9300 ?
C8 H8 . 0.9300 ?
C24 N3 . 1.355(4) ?
C24 C16 . 1.414(4) ?
C24 C23 . 1.451(4) ?
C16 C15 . 1.404(5) ?
C16 C17 . 1.424(5) ?
C23 N4 . 1.357(4) ?
C23 C19 . 1.408(5) ?
C19 C20 . 1.403(5) ?
C19 C18 . 1.434(5) ?
N3 C13 . 1.321(4) ?
N4 C22 . 1.333(5) ?
C18 C17 . 1.342(5) ?
C18 H18 . 0.9300 ?
C17 H17 . 0.9300 ?
C13 C14 . 1.387(5) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.359(5) ?
C14 H14 . 0.9300 ?
C20 C21 . 1.358(6) ?
C20 H20 . 0.9300 ?
C15 H15 . 0.9300 ?
C21 C22 . 1.387(6) ?
C21 H21 . 0.9300 ?
C22 H22 . 0.9300 ?
Cr1 O3 . 1.578(3) ?
Cr1 O2 . 1.597(3) ?
Cr1 O1 . 1.614(3) ?
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
O1W H1A N3 . 0.85 2.08 2.876(4) 156
O1W H1B O1 . 0.85 1.84 2.636(4) 154
