#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/88/1518860.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_1518860
loop_
_publ_author_name
'Dominik Hohne'
'Eberhardt Herdtweck'
'Alexander Pothig'
'Fritz E. Kuhn'
_publ_section_title
;
 Synthesis and characterization of dimeric and square-shaped
 dicarboxylate-bridged dimolybdenum(II) coordination compounds
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              210
_journal_page_last               215
_journal_volume                  424
_journal_year                    2015
_chemical_formula_moiety         'C36 H42 Br4 Mo4 N14 O4, 6(B F4)'
_chemical_formula_sum            'C36 H42 B6 Br4 F24 Mo4 N14 O4'
_chemical_formula_weight         1959.06
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                93.187(5)
_cell_angle_beta                 103.746(5)
_cell_angle_gamma                118.080(4)
_cell_formula_units_Z            1
_cell_length_a                   11.3474(11)
_cell_length_b                   11.7560(11)
_cell_length_c                   17.0657(16)
_cell_measurement_reflns_used    9647
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      1.25
_cell_volume                     1913.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2010)'
_computing_publication_material  'PLATON (Spek, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57939
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0552P)²+1.9991P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                6046
_reflns_number_total             7000
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ICA-2015-424-210-215-1.cif
_cod_data_source_block           2
_cod_database_code               1518860
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Mo1 Mo Uani 0.26167(3) 0.64806(3) 0.24875(2) 1.000 0.0187(1) . .
Mo2 Mo Uani 0.29709(3) 0.83727(3) 0.30178(2) 1.000 0.0188(1) . .
Br1 Br Uani 0.33574(4) 0.71766(3) 0.55731(2) 1.000 0.0252(1) . .
Br2 Br Uani 0.18525(4) 0.55646(3) 0.69209(2) 1.000 0.0244(1) . .
O1 O Uani 0.1476(2) 0.5575(2) 0.32870(14) 1.000 0.0211(7) . .
O2 O Uani 0.1815(2) 0.7512(2) 0.38226(14) 1.000 0.0194(7) . .
N1 N Uani 0.4199(3) 0.9640(3) 0.23241(19) 1.000 0.0259(9) . .
N2 N Uani 0.4933(3) 0.9015(3) 0.39274(18) 1.000 0.0227(9) . .
N3 N Uani 0.1250(3) 0.8445(3) 0.22208(19) 1.000 0.0241(9) . .
N4 N Uani 0.3824(3) 0.7071(3) 0.16409(18) 1.000 0.0235(9) . .
N5 N Uani 0.4300(3) 0.6360(3) 0.33001(18) 1.000 0.0235(9) . .
N6 N Uani 0.0724(3) 0.5886(3) 0.15316(18) 1.000 0.0241(9) . .
N7 N Uani 0.2085(3) 0.4224(3) 0.1862(2) 1.000 0.0297(10) . .
C1 C Uani 0.1341(4) 0.6288(3) 0.3801(2) 1.000 0.0208(10) . .
C2 C Uani 0.0643(3) 0.5647(3) 0.4426(2) 1.000 0.0180(10) . .
C3 C Uani 0.1422(3) 0.5931(3) 0.5249(2) 1.000 0.0194(10) . .
C4 C Uani 0.0788(3) 0.5277(3) 0.5823(2) 1.000 0.0191(10) . .
C5 C Uani 0.4808(4) 1.0314(4) 0.1941(2) 1.000 0.0297(12) . .
C6 C Uani 0.5578(5) 1.1150(4) 0.1430(3) 1.000 0.0476(16) . .
C7 C Uani 0.6098(4) 0.9488(3) 0.4283(2) 1.000 0.0252(11) . .
C8 C Uani 0.7571(4) 1.0084(4) 0.4693(2) 1.000 0.0336(12) . .
C9 C Uani 0.0485(4) 0.8678(3) 0.1804(2) 1.000 0.0257(11) . .
C10 C Uani -0.0508(4) 0.8964(4) 0.1267(3) 1.000 0.0416(14) . .
C11 C Uani 0.4512(4) 0.7378(3) 0.1215(2) 1.000 0.0245(11) . .
C12 C Uani 0.5393(4) 0.7793(4) 0.0668(2) 1.000 0.0297(12) . .
C13 C Uani 0.4935(4) 0.5938(3) 0.3640(2) 1.000 0.0230(11) . .
C14 C Uani 0.5723(4) 0.5347(4) 0.4062(2) 1.000 0.0324(12) . .
C15 C Uani -0.0292(4) 0.5457(3) 0.0998(2) 1.000 0.0253(11) . .
C16 C Uani -0.1570(4) 0.4896(4) 0.0313(2) 1.000 0.0323(12) . .
C17 C Uani 0.2215(4) 0.3409(4) 0.1560(2) 1.000 0.0307(12) . .
C18 C Uani 0.2346(6) 0.2365(4) 0.1170(3) 1.000 0.0482(16) . .
F1 F Uani 0.3519(2) 0.0647(2) 0.37915(14) 1.000 0.0321(7) . .
F2 F Uani 0.3448(3) 0.2396(2) 0.43688(17) 1.000 0.0461(8) . .
F3 F Uani 0.1491(3) 0.0682(3) 0.3479(2) 1.000 0.0610(10) . .
F4 F Uani 0.3284(4) 0.2073(3) 0.30196(19) 1.000 0.0737(14) . .
B1 B Uani 0.2922(5) 0.1472(5) 0.3652(3) 1.000 0.0361(16) . .
F5 F Uani 0.8553(3) 0.1218(3) 0.09677(18) 1.000 0.0674(11) . .
F6 F Uani 0.7043(3) 0.1447(3) -0.00508(17) 1.000 0.0536(10) . .
F7 F Uani 0.7920(4) 0.0152(3) -0.0327(2) 1.000 0.0740(13) . .
F8 F Uani 0.9317(3) 0.2350(3) -0.00006(18) 1.000 0.0599(10) . .
B2 B Uani 0.8220(5) 0.1300(4) 0.0152(3) 1.000 0.0328(14) . .
F9 F Uani 0.4768(3) 0.4904(3) 0.08532(16) 1.000 0.0530(9) . .
F10 F Uani 0.7124(3) 0.6232(2) 0.14132(18) 1.000 0.0546(10) . .
F11 F Uani 0.5758(3) 0.5298(3) 0.22269(15) 1.000 0.0520(10) . .
F12 F Uani 0.6155(3) 0.4055(2) 0.13787(17) 1.000 0.0477(9) . .
B3 B Uani 0.5941(5) 0.5126(5) 0.1469(3) 1.000 0.0336(14) . .
H61 H Uiso 0.56910 1.20260 0.15540 1.000 0.0710 calc R
H62 H Uiso 0.50570 1.07610 0.08480 1.000 0.0710 calc R
H63 H Uiso 0.65020 1.12220 0.15460 1.000 0.0710 calc R
H81 H Uiso 0.77860 0.94110 0.48790 1.000 0.0500 calc R
H82 H Uiso 0.78370 1.07560 0.51680 1.000 0.0500 calc R
H83 H Uiso 0.80960 1.04930 0.43110 1.000 0.0500 calc R
H101 H Uiso -0.03030 0.90790 0.07410 1.000 0.0620 calc R
H102 H Uiso -0.04270 0.97720 0.15270 1.000 0.0620 calc R
H103 H Uiso -0.14610 0.82330 0.11700 1.000 0.0620 calc R
H121 H Uiso 0.48980 0.79480 0.01680 1.000 0.0440 calc R
H122 H Uiso 0.56000 0.71040 0.05200 1.000 0.0440 calc R
H123 H Uiso 0.62690 0.86060 0.09490 1.000 0.0440 calc R
H141 H Uiso 0.50830 0.45340 0.42070 1.000 0.0490 calc R
H142 H Uiso 0.64340 0.59630 0.45630 1.000 0.0490 calc R
H143 H Uiso 0.61800 0.51470 0.36990 1.000 0.0490 calc R
H161 H Uiso -0.22920 0.49780 0.04920 1.000 0.0490 calc R
H162 H Uiso -0.18970 0.39650 0.01260 1.000 0.0490 calc R
H163 H Uiso -0.13850 0.53660 -0.01390 1.000 0.0490 calc R
H181 H Uiso 0.26640 0.19540 0.15920 1.000 0.0720 calc R
H182 H Uiso 0.30270 0.27300 0.08640 1.000 0.0720 calc R
H183 H Uiso 0.14350 0.17050 0.07920 1.000 0.0720 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
C C 0.0033 0.0016 '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
Mo2 Mo1 O1 90.81(6) . . yes
Mo2 Mo1 N4 99.81(9) . . yes
Mo2 Mo1 N5 102.08(9) . . yes
Mo2 Mo1 N6 98.19(9) . . yes
Mo2 Mo1 N7 177.38(9) . . yes
O1 Mo1 N4 168.75(11) . . yes
O1 Mo1 N5 85.64(11) . . yes
O1 Mo1 N6 90.68(11) . . yes
O1 Mo1 N7 87.45(10) . . yes
N4 Mo1 N5 88.49(13) . . yes
N4 Mo1 N6 91.47(13) . . yes
N4 Mo1 N7 82.06(12) . . yes
N5 Mo1 N6 159.43(12) . . yes
N5 Mo1 N7 79.75(12) . . yes
N6 Mo1 N7 79.88(12) . . yes
Mo1 Mo2 O2 90.78(6) . . yes
Mo1 Mo2 N1 101.77(9) . . yes
Mo1 Mo2 N2 98.04(9) . . yes
Mo1 Mo2 N3 101.40(9) . . yes
O2 Mo2 N1 167.45(11) . . yes
O2 Mo2 N2 93.05(11) . . yes
O2 Mo2 N3 91.79(11) . . yes
N1 Mo2 N2 85.41(13) . . yes
N1 Mo2 N3 85.64(13) . . yes
N2 Mo2 N3 159.89(12) . . yes
Mo1 O1 C1 118.1(2) . . yes
Mo2 O2 C1 117.7(2) . . yes
Mo2 N1 C5 177.5(4) . . yes
Mo2 N2 C7 165.0(3) . . yes
Mo2 N3 C9 169.5(3) . . yes
Mo1 N4 C11 176.9(3) . . yes
Mo1 N5 C13 160.9(3) . . yes
Mo1 N6 C15 173.4(3) . . yes
Mo1 N7 C17 160.7(3) . . yes
O1 C1 O2 122.5(3) . . yes
O1 C1 C2 117.4(3) . . yes
O2 C1 C2 120.0(3) . . yes
C1 C2 C3 120.5(3) . . no
C1 C2 C4 119.9(3) . 2_566 no
C3 C2 C4 119.6(3) . 2_566 no
Br1 C3 C2 119.0(3) . . yes
Br1 C3 C4 120.5(3) . . yes
C2 C3 C4 120.5(3) . . no
Br2 C4 C3 120.9(3) . . yes
Br2 C4 C2 119.1(2) . 2_566 yes
C2 C4 C3 119.9(3) 2_566 . no
N1 C5 C6 178.4(4) . . yes
N2 C7 C8 177.4(4) . . yes
N3 C9 C10 179.5(4) . . yes
N4 C11 C12 179.0(4) . . yes
N5 C13 C14 178.0(4) . . yes
N6 C15 C16 178.8(5) . . yes
N7 C17 C18 178.7(5) . . yes
C5 C6 H61 109.00 . . no
C5 C6 H62 109.00 . . no
C5 C6 H63 109.00 . . no
H61 C6 H62 109.00 . . no
H61 C6 H63 110.00 . . no
H62 C6 H63 110.00 . . no
C7 C8 H81 109.00 . . no
C7 C8 H82 110.00 . . no
C7 C8 H83 109.00 . . no
H81 C8 H82 110.00 . . no
H81 C8 H83 109.00 . . no
H82 C8 H83 109.00 . . no
C9 C10 H101 109.00 . . no
C9 C10 H102 110.00 . . no
C9 C10 H103 109.00 . . no
H101 C10 H102 109.00 . . no
H101 C10 H103 109.00 . . no
H102 C10 H103 110.00 . . no
C11 C12 H121 109.00 . . no
C11 C12 H122 110.00 . . no
C11 C12 H123 109.00 . . no
H121 C12 H122 109.00 . . no
H121 C12 H123 109.00 . . no
H122 C12 H123 110.00 . . no
C13 C14 H141 109.00 . . no
C13 C14 H142 109.00 . . no
C13 C14 H143 110.00 . . no
H141 C14 H142 109.00 . . no
H141 C14 H143 109.00 . . no
H142 C14 H143 109.00 . . no
C15 C16 H161 109.00 . . no
C15 C16 H162 109.00 . . no
C15 C16 H163 110.00 . . no
H161 C16 H162 109.00 . . no
H161 C16 H163 110.00 . . no
H162 C16 H163 110.00 . . no
C17 C18 H181 109.00 . . no
C17 C18 H182 109.00 . . no
C17 C18 H183 109.00 . . no
H181 C18 H182 109.00 . . no
H181 C18 H183 109.00 . . no
H182 C18 H183 110.00 . . no
F1 B1 F2 108.0(4) . . yes
F1 B1 F3 107.1(4) . . yes
F1 B1 F4 108.6(5) . . yes
F2 B1 F3 109.9(5) . . yes
F2 B1 F4 110.6(4) . . yes
F3 B1 F4 112.4(4) . . yes
F5 B2 F6 109.4(4) . . yes
F5 B2 F7 109.2(4) . . yes
F5 B2 F8 110.5(4) . . yes
F6 B2 F7 108.8(4) . . yes
F6 B2 F8 109.5(4) . . yes
F7 B2 F8 109.4(4) . . yes
F9 B3 F10 110.2(4) . . yes
F9 B3 F11 109.8(5) . . yes
F9 B3 F12 109.8(4) . . yes
F10 B3 F11 109.8(4) . . yes
F10 B3 F12 107.7(5) . . yes
F11 B3 F12 109.5(4) . . yes
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
Mo1 Mo2 2.1656(5) . yes
Mo1 O1 2.091(2) . yes
Mo1 N4 2.145(3) . yes
Mo1 N5 2.147(4) . yes
Mo1 N6 2.135(3) . yes
Mo1 N7 2.533(3) . yes
Mo2 O2 2.096(2) . yes
Mo2 N1 2.142(3) . yes
Mo2 N2 2.140(3) . yes
Mo2 N3 2.140(4) . yes
Br1 C3 1.892(4) . yes
Br2 C4 1.885(3) . yes
F1 B1 1.423(6) . yes
F2 B1 1.388(6) . yes
F3 B1 1.382(7) . yes
F4 B1 1.362(6) . yes
F5 B2 1.375(6) . yes
F6 B2 1.392(7) . yes
F7 B2 1.385(6) . yes
F8 B2 1.373(6) . yes
F9 B3 1.386(7) . yes
F10 B3 1.390(6) . yes
F11 B3 1.377(6) . yes
F12 B3 1.397(6) . yes
O1 C1 1.264(5) . yes
O2 C1 1.272(4) . yes
N1 C5 1.136(5) . yes
N2 C7 1.146(6) . yes
N3 C9 1.134(5) . yes
N4 C11 1.141(5) . yes
N5 C13 1.128(5) . yes
N6 C15 1.147(5) . yes
N7 C17 1.149(6) . yes
C1 C2 1.504(5) . no
C2 C3 1.395(5) . no
C2 C4 1.399(5) 2_566 no
C3 C4 1.402(5) . no
C5 C6 1.463(6) . no
C7 C8 1.436(6) . no
C9 C10 1.457(7) . no
C11 C12 1.464(6) . no
C13 C14 1.461(6) . no
C15 C16 1.454(6) . no
C17 C18 1.449(7) . no
C6 H63 0.9800 . no
C6 H62 0.9800 . no
C6 H61 0.9800 . no
C8 H82 0.9800 . no
C8 H83 0.9800 . no
C8 H81 0.9800 . no
C10 H101 0.9800 . no
C10 H102 0.9800 . no
C10 H103 0.9800 . no
C12 H122 0.9800 . no
C12 H123 0.9800 . no
C12 H121 0.9800 . no
C14 H141 0.9800 . no
C14 H142 0.9800 . no
C14 H143 0.9800 . no
C16 H161 0.9800 . no
C16 H163 0.9800 . no
C16 H162 0.9800 . no
C18 H182 0.9800 . no
C18 H183 0.9800 . no
C18 H181 0.9800 . no
