#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:34:15 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179536 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/05/4500556.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_4500556
loop_
_publ_author_name
'Singh, Monika'
'Ramanan, Arunachalam'
_publ_section_title
;
 Crystal Engineering of Polyoxomolybdates Based Metal--Organic Solids: The
 Case of Chromium Molybdate Cluster Based Metal Complexes and Coordination
 Polymers
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3381
_journal_paper_doi               10.1021/cg101695w
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety
'Cr Mo6 O24, C12 H8 N2 Ni O8, 2(C6 H6 N O2), 12(O)'
_chemical_formula_sum            'C24 H20 Cr Mo6 N4 Ni O48'
_chemical_formula_weight         1818.77
_chemical_name_common            anderson
_chemical_name_systematic
;  
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXTL-NT2000 ver.6.12'
_cell_angle_alpha                102.363(2)
_cell_angle_beta                 111.815(3)
_cell_angle_gamma                107.759(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5998(12)
_cell_length_b                   11.8436(14)
_cell_length_c                   13.1423(16)
_cell_measurement_reflns_used    2163
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.29
_cell_volume                     1355.0(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.899
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6312
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.998
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             880.0
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.921
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0647
_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)+(0.0459P)²+10.8889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                3733
_reflns_number_total             4766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101695w_si_002.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4500556
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cr1 Cr 0.0000 0.5000 0.5000 0.0246(4) Uani 1 2 d S
Mo1 Mo 0.11931(9) 0.29091(7) 0.58305(8) 0.0331(2) Uani 1 1 d .
Mo2 Mo 0.05386(9) 0.29788(7) 0.31858(7) 0.0333(2) Uani 1 1 d .
Mo3 Mo -0.06272(9) 0.50869(7) 0.23395(7) 0.0318(2) Uani 1 1 d .
Ni1 Ni 0.5000 1.0000 0.0000 0.0495(5) Uani 1 2 d S
O1 O 0.0040(7) 0.3183(5) 0.6665(5) 0.0315(14) Uani 1 1 d .
O2 O 0.2814(8) 0.3153(7) 0.6980(7) 0.058(2) Uani 1 1 d .
O3 O 0.0187(8) 0.1293(6) 0.5188(7) 0.0517(19) Uani 1 1 d .
O4 O 0.1958(7) 0.3251(5) 0.4767(6) 0.0353(15) Uani 1 1 d .
O5 O -0.0426(8) 0.1355(6) 0.2594(6) 0.0504(19) Uani 1 1 d .
O6 O 0.1759(8) 0.3317(7) 0.2635(7) 0.0535(19) Uani 1 1 d .
O7 O -0.1059(7) 0.3324(5) 0.2153(5) 0.0349(15) Uani 1 1 d .
O8 O 0.0666(8) 0.5455(7) 0.1841(6) 0.0498(18) Uani 1 1 d .
O9 O -0.2263(9) 0.4817(7) 0.1204(6) 0.059(2) Uani 1 1 d .
O10 O -0.1630(6) 0.4993(5) 0.3617(5) 0.0258(13) Uani 1 1 d .
O11 O 0.1027(6) 0.5069(5) 0.4022(5) 0.0252(13) Uani 1 1 d .
O12 O -0.0571(6) 0.3169(5) 0.4384(5) 0.0272(13) Uani 1 1 d .
O13 O 0.3381(7) 0.9399(6) 0.0412(6) 0.0440(17) Uani 1 1 d .
O14 O 0.3173(8) 1.1098(7) 0.1316(7) 0.0518(19) Uani 1 1 d .
O15 O 0.6232(8) 1.1563(6) 0.1435(6) 0.052(2) Uani 1 1 d .
O16 O 0.5924(8) 0.9019(7) 0.0834(6) 0.0540(19) Uani 1 1 d .
O17 O 0.3434(7) 0.8198(6) 0.6373(6) 0.0477(18) Uani 1 1 d .
H17 H 0.2700 0.7542 0.6179 0.072 Uiso 1 1 calc R
O18 O 0.3739(7) 0.6984(6) 0.5026(6) 0.0487(18) Uani 1 1 d .
N1 N -0.1358(10) 0.7462(9) 0.0485(8) 0.050(2) Uani 1 1 d .
N2 N 0.7870(8) 1.1138(7) 0.6390(6) 0.0356(19) Uani 1 1 d .
H2 H 0.8608 1.1778 0.6472 0.043 Uiso 1 1 calc R
C1 C 0.2771(10) 0.9950(8) 0.0849(7) 0.031(2) Uani 1 1 d D
C2 C 0.1318(10) 0.9049(9) 0.0740(7) 0.032(2) Uani 1 1 d D
C3 C 0.0477(11) 0.9534(10) 0.1150(9) 0.044(2) Uani 1 1 d .
H3 H 0.0816 1.0409 0.1516 0.053 Uiso 1 1 calc R
C4 C -0.0842(12) 0.8706(11) 0.1004(9) 0.048(3) Uani 1 1 d .
H4 H -0.1401 0.9027 0.1279 0.058 Uiso 1 1 calc R
C5 C -0.0559(13) 0.6963(10) 0.0119(9) 0.053(3) Uani 1 1 d .
H5 H -0.0921 0.6081 -0.0221 0.064 Uiso 1 1 calc R
C6 C 0.0776(12) 0.7729(10) 0.0238(9) 0.046(3) Uani 1 1 d .
H6 H 0.1327 0.7373 -0.0015 0.055 Uiso 1 1 calc R
C7 C 0.4111(10) 0.7976(8) 0.5806(8) 0.033(2) Uani 1 1 d .
C8 C 0.5503(10) 0.9105(8) 0.6072(7) 0.028(2) Uani 1 1 d .
C9 C 0.5697(10) 1.0334(8) 0.6582(7) 0.032(2) Uani 1 1 d .
H9 H 0.5025 1.0475 0.6831 0.039 Uiso 1 1 calc R
C10 C 0.6904(12) 1.1354(8) 0.6720(8) 0.040(2) Uani 1 1 d .
H10 H 0.7032 1.2186 0.7043 0.048 Uiso 1 1 calc R
C11 C 0.7745(11) 0.9959(10) 0.5932(8) 0.042(2) Uani 1 1 d .
H11 H 0.8463 0.9846 0.5730 0.050 Uiso 1 1 calc R
C12 C 0.6555(10) 0.8916(9) 0.5763(8) 0.039(2) Uani 1 1 d .
H12 H 0.6458 0.8095 0.5444 0.046 Uiso 1 1 calc R
O1W O 0.5701(12) 0.614(2) 0.9770(15) 0.222(11) Uani 1 1 d .
O2W O 0.500(2) 0.4679(17) 0.588(3) 0.282(18) Uani 1 1 d .
O3W O 0.5268(9) 0.3730(8) 0.2471(8) 0.072(3) Uani 1 1 d .
O4W O 0.384(2) 0.600(2) 0.246(3) 0.265(13) Uani 1 1 d .
O5W O 0.421(3) 0.693(2) 0.110(3) 0.316(16) Uani 1 1 d .
O6W O 0.7337(10) 0.9387(8) 0.3071(7) 0.074(3) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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'
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
O12 Cr1 O12 180.000(1) . 2_566
O12 Cr1 O11 95.9(2) . 2_566
O12 Cr1 O11 84.1(2) 2_566 2_566
O12 Cr1 O11 84.1(2) . .
O12 Cr1 O11 95.9(2) 2_566 .
O11 Cr1 O11 180.000(1) 2_566 .
O12 Cr1 O10 95.7(2) . .
O12 Cr1 O10 84.3(2) 2_566 .
O11 Cr1 O10 96.5(2) 2_566 .
O11 Cr1 O10 83.5(2) . .
O12 Cr1 O10 84.3(2) . 2_566
O12 Cr1 O10 95.7(2) 2_566 2_566
O11 Cr1 O10 83.5(2) 2_566 2_566
O11 Cr1 O10 96.5(2) . 2_566
O10 Cr1 O10 180.000(1) . 2_566
O2 Mo1 O3 105.1(4) . .
O2 Mo1 O4 98.7(3) . .
O3 Mo1 O4 101.5(3) . .
O2 Mo1 O1 100.3(3) . .
O3 Mo1 O1 95.0(3) . .
O4 Mo1 O1 150.6(2) . .
O2 Mo1 O12 163.5(3) . .
O3 Mo1 O12 90.6(3) . .
O4 Mo1 O12 72.9(2) . .
O1 Mo1 O12 82.8(2) . .
O2 Mo1 O10 94.5(3) . 2_566
O3 Mo1 O10 158.1(3) . 2_566
O4 Mo1 O10 84.8(2) . 2_566
O1 Mo1 O10 71.5(2) . 2_566
O12 Mo1 O10 71.00(19) . 2_566
O6 Mo2 O5 105.6(3) . .
O6 Mo2 O4 98.1(3) . .
O5 Mo2 O4 101.4(3) . .
O6 Mo2 O7 100.9(3) . .
O5 Mo2 O7 96.2(3) . .
O4 Mo2 O7 149.5(2) . .
O6 Mo2 O11 94.1(3) . .
O5 Mo2 O11 158.5(3) . .
O4 Mo2 O11 83.8(2) . .
O7 Mo2 O11 71.3(2) . .
O6 Mo2 O12 161.4(3) . .
O5 Mo2 O12 91.9(3) . .
O4 Mo2 O12 71.7(2) . .
O7 Mo2 O12 83.2(2) . .
O11 Mo2 O12 69.78(18) . .
O9 Mo3 O8 104.8(4) . .
O9 Mo3 O7 97.3(3) . .
O8 Mo3 O7 102.2(3) . .
O9 Mo3 O1 100.7(3) . 2_566
O8 Mo3 O1 96.9(3) . 2_566
O7 Mo3 O1 149.3(2) . 2_566
O9 Mo3 O11 161.3(3) . .
O8 Mo3 O11 92.8(3) . .
O7 Mo3 O11 72.2(2) . .
O1 Mo3 O11 83.2(2) 2_566 .
O9 Mo3 O10 93.2(3) . .
O8 Mo3 O10 160.3(3) . .
O7 Mo3 O10 82.9(2) . .
O1 Mo3 O10 71.5(2) 2_566 .
O11 Mo3 O10 70.47(19) . .
O13 Ni1 O13 180.000(1) . 2_675
O13 Ni1 O15 86.0(3) . 2_675
O13 Ni1 O15 94.0(3) 2_675 2_675
O13 Ni1 O15 94.0(3) . .
O13 Ni1 O15 86.0(3) 2_675 .
O15 Ni1 O15 180.000(1) 2_675 .
O13 Ni1 O16 87.8(3) . .
O13 Ni1 O16 92.2(3) 2_675 .
O15 Ni1 O16 88.9(3) 2_675 .
O15 Ni1 O16 91.1(3) . .
O13 Ni1 O16 92.2(3) . 2_675
O13 Ni1 O16 87.8(3) 2_675 2_675
O15 Ni1 O16 91.1(3) 2_675 2_675
O15 Ni1 O16 88.9(3) . 2_675
O16 Ni1 O16 180.000(1) . 2_675
Mo3 O1 Mo1 118.2(3) 2_566 .
Mo1 O4 Mo2 118.0(3) . .
Mo3 O7 Mo2 117.3(3) . .
Cr1 O10 Mo1 101.7(2) . 2_566
Cr1 O10 Mo3 102.1(2) . .
Mo1 O10 Mo3 94.32(19) 2_566 .
Cr1 O11 Mo3 103.9(2) . .
Cr1 O11 Mo2 103.0(2) . .
Mo3 O11 Mo2 93.8(2) . .
Cr1 O12 Mo1 103.0(2) . .
Cr1 O12 Mo2 103.1(2) . .
Mo1 O12 Mo2 92.6(2) . .
C1 O13 Ni1 133.0(6) . .
C7 O17 H17 109.5 . .
C4 N1 C5 120.6(9) . .
C10 N2 C11 122.6(8) . .
C10 N2 H2 118.7 . .
C11 N2 H2 118.7 . .
O14 C1 O13 128.6(9) . .
O14 C1 C2 117.6(8) . .
O13 C1 C2 113.8(8) . .
C6 C2 C3 117.8(9) . .
C6 C2 C1 122.0(8) . .
C3 C2 C1 120.2(8) . .
C4 C3 C2 118.8(10) . .
C4 C3 H3 120.6 . .
C2 C3 H3 120.6 . .
N1 C4 C3 122.2(10) . .
N1 C4 H4 118.9 . .
C3 C4 H4 118.9 . .
N1 C5 C6 120.6(10) . .
N1 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C5 C6 C2 119.9(10) . .
C5 C6 H6 120.1 . .
C2 C6 H6 120.1 . .
O18 C7 O17 127.7(8) . .
O18 C7 C8 116.5(8) . .
O17 C7 C8 115.6(8) . .
C9 C8 C12 119.4(8) . .
C9 C8 C7 120.1(8) . .
C12 C8 C7 120.4(8) . .
C8 C9 C10 119.3(9) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
N2 C10 C9 119.6(9) . .
N2 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
N2 C11 C12 119.9(9) . .
N2 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C11 C12 C8 119.1(9) . .
C11 C12 H12 120.4 . .
C8 C12 H12 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O12 1.952(5) .
Cr1 O12 1.952(5) 2_566
Cr1 O11 1.969(5) 2_566
Cr1 O11 1.969(5) .
Cr1 O10 1.985(5) .
Cr1 O10 1.985(5) 2_566
Mo1 O2 1.703(7) .
Mo1 O3 1.705(7) .
Mo1 O4 1.913(6) .
Mo1 O1 1.972(6) .
Mo1 O12 2.272(6) .
Mo1 O10 2.278(5) 2_566
Mo2 O6 1.692(7) .
Mo2 O5 1.708(6) .
Mo2 O4 1.944(7) .
Mo2 O7 1.956(6) .
Mo2 O11 2.288(5) .
Mo2 O12 2.302(6) .
Mo3 O9 1.695(7) .
Mo3 O8 1.710(7) .
Mo3 O7 1.935(6) .
Mo3 O1 1.941(6) 2_566
Mo3 O11 2.264(6) .
Mo3 O10 2.301(6) .
Ni1 O13 1.963(6) .
Ni1 O13 1.963(6) 2_675
Ni1 O15 1.972(6) 2_675
Ni1 O15 1.972(6) .
Ni1 O16 1.988(7) .
Ni1 O16 1.988(7) 2_675
O1 Mo3 1.941(6) 2_566
O10 Mo1 2.278(5) 2_566
O13 C1 1.243(11) .
O14 C1 1.226(11) .
O17 C7 1.253(11) .
O17 H17 0.8200 .
O18 C7 1.220(11) .
N1 C4 1.318(14) .
N1 C5 1.337(14) .
N2 C10 1.321(13) .
N2 C11 1.341(13) .
N2 H2 0.8600 .
C1 C2 1.517(12) .
C2 C6 1.392(13) .
C2 C3 1.397(14) .
C3 C4 1.355(14) .
C3 H3 0.9300 .
C4 H4 0.9300 .
C5 C6 1.357(14) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.516(12) .
C8 C9 1.381(12) .
C8 C12 1.381(13) .
C9 C10 1.385(13) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.374(13) .
C11 H11 0.9300 .
C12 H12 0.9300 .
