#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/52/4505221.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_4505221
loop_
_publ_author_name
'Mukhopadhyay, Uday'
'Bernal, Ivan'
_publ_section_title
;
 Self-Assembled Hexameric Water Clusters Stabilized by a Cyano-Bridged
 Trimetallic Complex
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1687
_journal_paper_doi               10.1021/cg0501940
_journal_volume                  5
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H30 Cu1 Mo1 N8 O3'
_chemical_formula_sum            'C14 H30 Cu Mo0.5 N8 O3'
_chemical_formula_weight         469.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_cell_angle_alpha                90
_cell_angle_beta                 95.80(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.735(5)
_cell_length_b                   9.323(3)
_cell_length_c                   20.978(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     4034.5(19)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.027241
_diffrn_orient_matrix_UB_12      -0.028023
_diffrn_orient_matrix_UB_13      0.040117
_diffrn_orient_matrix_UB_21      0.03237
_diffrn_orient_matrix_UB_22      0.075343
_diffrn_orient_matrix_UB_23      -0.008363
_diffrn_orient_matrix_UB_31      -0.023663
_diffrn_orient_matrix_UB_32      0.071013
_diffrn_orient_matrix_UB_33      0.024829
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4191
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.4
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.411
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0366P)²+3.2756P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.062
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                3268
_reflns_number_total             3964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0501940si20050712_101701.cif
_cod_data_source_block
;
;
_cod_original_cell_volume        4034.7(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C14 H30 Cu Mo0.50 N8 O3'
_cod_database_code               4505221
#BEGIN Tags that were not found in dictionaries:
_diffrn_standards_decay_corr_max 1
_diffrn_standards_decay_corr_min 1
#END Tags that were not found in dictionaries
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
Mo1 Mo 0.5 -0.23450(3) 0.75 0.01789(8) Uani 1 2 d S
Cu1 Cu 0.602243(13) 0.19581(3) 0.624500(13) 0.02327(9) Uani 1 1 d .
N1 N 0.54027(13) 0.3414(3) 0.58126(13) 0.0385(5) Uani 1 1 d .
N2 N 0.62401(10) 0.1054(2) 0.53962(9) 0.0294(4) Uani 1 1 d .
N3 N 0.69228(9) 0.0988(2) 0.64214(9) 0.0273(4) Uani 1 1 d .
N4 N 0.61045(15) 0.3162(3) 0.70458(11) 0.0410(6) Uani 1 1 d .
N5 N 0.53914(10) 0.0353(2) 0.65852(11) 0.0344(5) Uani 1 1 d .
N6 N 0.63867(11) -0.1151(3) 0.82347(12) 0.0452(6) Uani 1 1 d .
N7 N 0.55983(13) -0.5119(3) 0.83481(13) 0.0529(7) Uani 1 1 d .
N8 N 0.60679(12) -0.3574(2) 0.65664(12) 0.0464(6) Uani 1 1 d .
C1 C 0.50269(14) 0.3007(3) 0.52051(15) 0.0422(7) Uani 1 1 d .
C2 C 0.54587(16) 0.2593(4) 0.46986(14) 0.0489(8) Uani 1 1 d .
C3 C 0.57826(15) 0.1152(4) 0.48046(13) 0.0434(7) Uani 1 1 d .
C4 C 0.63802(14) -0.0466(3) 0.55653(13) 0.0379(6) Uani 1 1 d .
C5 C 0.68258(14) -0.0498(3) 0.61875(14) 0.0367(6) Uani 1 1 d .
C6 C 0.68686(13) 0.1764(3) 0.53075(13) 0.0351(6) Uani 1 1 d .
C7 C 0.72821(13) 0.1770(3) 0.59526(13) 0.0357(6) Uani 1 1 d .
C8 C 0.72776(15) 0.0991(3) 0.70704(14) 0.0399(6) Uani 1 1 d .
C9 C 0.72157(16) 0.2367(4) 0.74291(15) 0.0468(7) Uani 1 1 d .
C10 C 0.65427(17) 0.2640(3) 0.76033(13) 0.0447(7) Uani 1 1 d .
C11 C 0.52390(11) -0.0568(2) 0.68981(11) 0.0241(5) Uani 1 1 d .
C13 C 0.54081(12) -0.4138(3) 0.80566(12) 0.0317(5) Uani 1 1 d .
C12 C 0.59077(11) -0.1578(3) 0.79870(11) 0.0289(5) Uani 1 1 d .
C14 C 0.57013(12) -0.3129(2) 0.68906(12) 0.0302(5) Uani 1 1 d .
OW1 O 0.66822(11) 0.5374(2) 0.55316(10) 0.0526(5) Uani 1 1 d .
OW2 O 0.84599(12) -0.1414(3) 0.56922(11) 0.0743(7) Uani 1 1 d .
OW3 O 0.79597(12) 0.5985(3) 0.59732(12) 0.0680(7) Uani 1 1 d .
H1 H 0.5141(16) 0.368(4) 0.6061(16) 0.052(10) Uiso 1 1 d .
H2 H 0.5639(16) 0.406(4) 0.5762(16) 0.052(10) Uiso 1 1 d .
H3 H 0.4761(14) 0.216(3) 0.5277(15) 0.045(8) Uiso 1 1 d .
H4 H 0.4744(13) 0.384(3) 0.5051(14) 0.043(8) Uiso 1 1 d .
H5 H 0.5221(19) 0.258(4) 0.4301(19) 0.071(11) Uiso 1 1 d .
H6 H 0.5758(17) 0.338(4) 0.4672(16) 0.058(10) Uiso 1 1 d .
H7 H 0.5426(15) 0.037(3) 0.4858(14) 0.052(9) Uiso 1 1 d .
H8 H 0.6002(14) 0.090(3) 0.4450(15) 0.048(8) Uiso 1 1 d .
H9 H 0.5952(13) -0.095(3) 0.5630(12) 0.035(7) Uiso 1 1 d .
H10 H 0.6552(16) -0.094(4) 0.5251(16) 0.059(10) Uiso 1 1 d .
H11 H 0.6636(12) -0.103(3) 0.6472(12) 0.026(6) Uiso 1 1 d .
H12 H 0.7208(16) -0.084(3) 0.6125(15) 0.050(9) Uiso 1 1 d .
H13 H 0.6784(13) 0.272(3) 0.5158(13) 0.035(7) Uiso 1 1 d .
H14 H 0.7049(13) 0.122(3) 0.4988(13) 0.037(7) Uiso 1 1 d .
H15 H 0.7335(13) 0.273(3) 0.6110(14) 0.039(8) Uiso 1 1 d .
H16 H 0.7698(13) 0.134(3) 0.5939(12) 0.033(7) Uiso 1 1 d .
H17 H 0.7102(13) 0.026(3) 0.7301(13) 0.039(8) Uiso 1 1 d .
H18 H 0.7701(15) 0.077(3) 0.7034(14) 0.047(9) Uiso 1 1 d .
H19 H 0.7362(17) 0.312(4) 0.7196(17) 0.060(10) Uiso 1 1 d .
H20 H 0.7529(18) 0.230(4) 0.7831(19) 0.072(11) Uiso 1 1 d .
H21 H 0.6329(13) 0.181(3) 0.7724(14) 0.037(8) Uiso 1 1 d .
H22 H 0.6545(16) 0.327(4) 0.7963(17) 0.061(10) Uiso 1 1 d .
H23 H 0.5693(18) 0.315(4) 0.7146(18) 0.064(12) Uiso 1 1 d .
H24 H 0.624(2) 0.401(5) 0.6958(19) 0.083(14) Uiso 1 1 d .
HW1 H 0.6598 0.5822 0.5151 0.05 Uiso 1 1 d .
HW2 H 0.6448 0.5898 0.5793 0.05 Uiso 1 1 d .
HW3 H 0.7738 0.5602 0.581 0.05 Uiso 1 1 d .
HW4 H 0.8144 0.5256 0.6216 0.05 Uiso 1 1 d .
HW5 H 0.8818 -0.1891 0.565 0.05 Uiso 1 1 d .
HW6 H 0.8781 -0.1008 0.6018 0.05 Uiso 1 1 d .
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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
C14 Mo1 C14 140.42(12) . 2_656
C14 Mo1 C13 78.92(9) . .
C14 Mo1 C13 70.65(9) 2_656 .
C14 Mo1 C13 70.65(9) . 2_656
C14 Mo1 C13 78.92(9) 2_656 2_656
C13 Mo1 C13 78.72(14) . 2_656
C14 Mo1 C12 77.65(9) . .
C14 Mo1 C12 115.90(10) 2_656 .
C13 Mo1 C12 74.15(10) . .
C13 Mo1 C12 141.49(9) 2_656 .
C14 Mo1 C12 115.90(10) . 2_656
C14 Mo1 C12 77.65(9) 2_656 2_656
C13 Mo1 C12 141.49(9) . 2_656
C13 Mo1 C12 74.15(10) 2_656 2_656
C12 Mo1 C12 141.54(13) . 2_656
C14 Mo1 C11 144.10(9) . 2_656
C14 Mo1 C11 72.95(9) 2_656 2_656
C13 Mo1 C11 112.08(9) . 2_656
C13 Mo1 C11 143.56(9) 2_656 2_656
C12 Mo1 C11 73.31(9) . 2_656
C12 Mo1 C11 77.55(9) 2_656 2_656
C14 Mo1 C11 72.95(9) . .
C14 Mo1 C11 144.10(9) 2_656 .
C13 Mo1 C11 143.56(9) . .
C13 Mo1 C11 112.08(9) 2_656 .
C12 Mo1 C11 77.55(9) . .
C12 Mo1 C11 73.31(9) 2_656 .
C11 Mo1 C11 80.49(12) 2_656 .
N4 Cu1 N1 89.79(11) . .
N4 Cu1 N2 160.30(11) . .
N1 Cu1 N2 94.11(10) . .
N4 Cu1 N3 95.48(10) . .
N1 Cu1 N3 153.31(10) . .
N2 Cu1 N3 72.79(8) . .
N4 Cu1 N5 96.54(11) . .
N1 Cu1 N5 103.61(11) . .
N2 Cu1 N5 101.27(9) . .
N3 Cu1 N5 101.76(8) . .
C1 N1 Cu1 118.14(18) . .
C4 N2 C3 110.5(2) . .
C4 N2 C6 107.6(2) . .
C3 N2 C6 111.2(2) . .
C4 N2 Cu1 103.82(15) . .
C3 N2 Cu1 121.30(17) . .
C6 N2 Cu1 101.36(15) . .
C5 N3 C8 110.2(2) . .
C5 N3 C7 107.5(2) . .
C8 N3 C7 111.9(2) . .
C5 N3 Cu1 105.06(16) . .
C8 N3 Cu1 121.21(17) . .
C7 N3 Cu1 99.83(15) . .
C10 N4 Cu1 117.81(18) . .
C11 N5 Cu1 157.3(2) . .
N1 C1 C2 112.1(3) . .
C1 C2 C3 114.3(2) . .
N2 C3 C2 114.5(2) . .
N2 C4 C5 108.1(2) . .
N3 C5 C4 108.5(2) . .
N2 C6 C7 108.1(2) . .
N3 C7 C6 108.1(2) . .
N3 C8 C9 113.8(2) . .
C10 C9 C8 113.3(3) . .
N4 C10 C9 111.9(3) . .
N5 C11 Mo1 177.2(2) . .
N7 C13 Mo1 176.9(3) . .
N6 C12 Mo1 178.6(2) . .
N8 C14 Mo1 178.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C14 2.158(3) .
Mo1 C14 2.158(3) 2_656
Mo1 C13 2.162(2) .
Mo1 C13 2.162(2) 2_656
Mo1 C12 2.170(3) .
Mo1 C12 2.170(3) 2_656
Mo1 C11 2.170(2) 2_656
Mo1 C11 2.170(2) .
Cu1 N4 2.013(2) .
Cu1 N1 2.020(2) .
Cu1 N2 2.061(2) .
Cu1 N3 2.074(2) .
Cu1 N5 2.156(2) .
N1 C1 1.475(4) .
N2 C4 1.483(3) .
N2 C3 1.487(3) .
N2 C6 1.490(3) .
N3 C5 1.477(3) .
N3 C8 1.481(3) .
N3 C7 1.484(3) .
N4 C10 1.489(4) .
N5 C11 1.145(3) .
N6 C12 1.145(3) .
N7 C13 1.148(3) .
N8 C14 1.148(3) .
C1 C2 1.507(5) .
C2 C3 1.509(5) .
C4 C5 1.521(4) .
C6 C7 1.527(4) .
C8 C9 1.500(4) .
C9 C10 1.499(5) .
