#------------------------------------------------------------------------------
#$Date: 2019-11-25 02:17:08 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239947 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/05/4350575.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_4350575
loop_
_publ_author_name
'Cotton, F. Albert'
'Liu, Chun Y.'
'Murillo, Carlos A.'
'Zhao, Qinliang'
_publ_section_title
;
 Strong electronic communication by direct metal-metal interaction in
 molecules with halide-bridged dimolybdenum pairs.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9493
_journal_page_last               9501
_journal_paper_doi               10.1021/ic061304a
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C60 H60 Br4 Mo4 N8 O8, 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H64 Br4 Cl4 Mo4 N8 O8'
_chemical_formula_weight         1894.41
_chemical_name_common            '[Mo2(DAniF)2]2Br4, 2CH2Cl2'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.568(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8343(19)
_cell_length_b                   12.405(2)
_cell_length_c                   23.934(4)
_cell_measurement_reflns_used    6503
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.38
_cell_volume                     3474.4(10)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'BRUKER SMART 1000'
_diffrn_measurement_method       ω-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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20862
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.217
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.675
_refine_diff_density_rms
'0.124 =============the end of compound 2=================== ============compound 2-PF6================================'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0424
_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)+(0.0456P)²+16.1554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                6958
_reflns_number_total             7900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061304asi20060715_074716.cif
_cod_data_source_block           xl
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4350575
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.50905(3) 0.16781(3) 0.018903(14) 0.02489(9) Uani 1 1 d .
Mo2 Mo 0.56237(3) 0.11054(3) -0.056359(15) 0.02575(9) Uani 1 1 d .
Br1 Br 0.31421(4) 0.06425(4) 0.024747(19) 0.03171(11) Uani 1 1 d .
Br2 Br 0.58985(4) 0.03246(4) 0.10034(2) 0.03895(12) Uani 1 1 d .
N1 N 0.6595(3) 0.2606(3) 0.03936(15) 0.0278(7) Uani 1 1 d .
N2 N 0.7157(3) 0.1944(3) -0.04125(15) 0.0299(8) Uani 1 1 d .
N3 N 0.4131(3) 0.2909(3) -0.02331(15) 0.0304(8) Uani 1 1 d .
N4 N 0.4725(3) 0.2334(3) -0.10502(15) 0.0313(8) Uani 1 1 d .
O1 O 0.7528(4) 0.5170(3) 0.23290(14) 0.0496(9) Uani 1 1 d .
O2 O 1.0554(3) 0.1236(4) -0.17591(16) 0.0571(11) Uani 1 1 d .
O3 O 0.0717(5) 0.4905(5) 0.0771(3) 0.0939(18) Uani 1 1 d .
O4 O 0.5140(5) 0.3451(4) -0.32727(18) 0.0716(14) Uani 1 1 d .
C10 C 0.7388(4) 0.2520(4) 0.00586(18) 0.0296(9) Uani 1 1 d .
H10A H 0.8101 0.2861 0.0153 0.035 Uiso 1 1 calc R
C11 C 0.6834(4) 0.3312(4) 0.08703(18) 0.0295(9) Uani 1 1 d .
C12 C 0.6325(4) 0.3115(4) 0.1350(2) 0.0384(11) Uani 1 1 d .
H12A H 0.5811 0.2536 0.1349 0.046 Uiso 1 1 calc R
C13 C 0.6562(5) 0.3754(4) 0.1826(2) 0.0424(11) Uani 1 1 d .
H13A H 0.6209 0.3611 0.2145 0.051 Uiso 1 1 calc R
C14 C 0.7321(4) 0.4609(4) 0.18318(19) 0.0353(10) Uani 1 1 d .
C15 C 0.7792(4) 0.4842(4) 0.1355(2) 0.0347(10) Uani 1 1 d .
H15A H 0.8287 0.5434 0.1354 0.042 Uiso 1 1 calc R
C16 C 0.7540(4) 0.4208(4) 0.08744(19) 0.0317(9) Uani 1 1 d .
H16A H 0.7851 0.4387 0.0547 0.038 Uiso 1 1 calc R
C17 C 0.8155(6) 0.6139(5) 0.2340(3) 0.0618(17) Uani 1 1 d .
H17A H 0.8237 0.6448 0.2717 0.093 Uiso 1 1 calc R
H17B H 0.7755 0.6644 0.2071 0.093 Uiso 1 1 calc R
H17C H 0.8906 0.5992 0.2241 0.093 Uiso 1 1 calc R
C21 C 0.8061(4) 0.1746(4) -0.07383(19) 0.0313(9) Uani 1 1 d .
C22 C 0.9129(4) 0.1418(4) -0.04932(19) 0.0372(10) Uani 1 1 d .
H22A H 0.9280 0.1319 -0.0100 0.045 Uiso 1 1 calc R
C23 C 0.9994(4) 0.1230(5) -0.0819(2) 0.0402(11) Uani 1 1 d .
H23A H 1.0724 0.1015 -0.0646 0.048 Uiso 1 1 calc R
C24 C 0.8680(5) 0.1653(5) -0.1649(2) 0.0459(13) Uani 1 1 d .
H24A H 0.8518 0.1723 -0.2044 0.055 Uiso 1 1 calc R
C25 C 0.9765(4) 0.1361(5) -0.1402(2) 0.0414(11) Uani 1 1 d .
C26 C 0.7831(4) 0.1844(4) -0.13264(19) 0.0393(11) Uani 1 1 d .
H26A H 0.7096 0.2040 -0.1501 0.047 Uiso 1 1 calc R
C27 C 1.1644(5) 0.0857(7) -0.1518(3) 0.068(2) Uani 1 1 d .
H27A H 1.2130 0.0802 -0.1809 0.102 Uiso 1 1 calc R
H27B H 1.1568 0.0153 -0.1352 0.102 Uiso 1 1 calc R
H27C H 1.1981 0.1356 -0.1228 0.102 Uiso 1 1 calc R
C30 C 0.4108(4) 0.3004(4) -0.07826(19) 0.0332(9) Uani 1 1 d .
H30A H 0.3659 0.3542 -0.0985 0.040 Uiso 1 1 calc R
C31 C 0.3301(4) 0.3503(4) 0.0019(2) 0.0368(10) Uani 1 1 d .
C32 C 0.3611(6) 0.4218(6) 0.0440(3) 0.0641(18) Uani 1 1 d .
H32A H 0.4386 0.4379 0.0561 0.077 Uiso 1 1 calc R
C33 C 0.2724(7) 0.4727(6) 0.0702(3) 0.074(2) Uani 1 1 d .
H33A H 0.2911 0.5240 0.0990 0.089 Uiso 1 1 calc R
C34 C 0.1623(6) 0.4459(6) 0.0527(3) 0.0653(19) Uani 1 1 d .
C35 C 0.1304(6) 0.3789(6) 0.0096(3) 0.0652(18) Uani 1 1 d .
H35A H 0.0527 0.3666 -0.0039 0.078 Uiso 1 1 calc R
C36 C 0.2136(5) 0.3293(5) -0.0142(3) 0.0538(15) Uani 1 1 d .
H36A H 0.1920 0.2783 -0.0429 0.065 Uiso 1 1 calc R
C37 C 0.0954(10) 0.5540(8) 0.1220(6) 0.131(5) Uani 1 1 d .
H37A H 0.0247 0.5783 0.1338 0.196 Uiso 1 1 calc R
H37B H 0.1388 0.6158 0.1124 0.196 Uiso 1 1 calc R
H37C H 0.1399 0.5142 0.1525 0.196 Uiso 1 1 calc R
C41 C 0.4806(4) 0.2586(4) -0.1622(2) 0.0362(10) Uani 1 1 d .
C42 C 0.4685(5) 0.1802(5) -0.2032(2) 0.0508(14) Uani 1 1 d .
H42A H 0.4535 0.1087 -0.1936 0.061 Uiso 1 1 calc R
C43 C 0.4783(5) 0.2061(6) -0.2596(2) 0.0574(16) Uani 1 1 d .
H43A H 0.4695 0.1524 -0.2876 0.069 Uiso 1 1 calc R
C44 C 0.5010(5) 0.3109(5) -0.2733(2) 0.0501(14) Uani 1 1 d .
C45 C 0.5146(6) 0.3900(5) -0.2330(3) 0.0538(14) Uani 1 1 d .
H45A H 0.5310 0.4612 -0.2427 0.065 Uiso 1 1 calc R
C46 C 0.5040(5) 0.3638(5) -0.1780(2) 0.0472(13) Uani 1 1 d .
H46A H 0.5127 0.4182 -0.1504 0.057 Uiso 1 1 calc R
C47 C 0.4958(10) 0.2696(9) -0.3701(3) 0.115(4) Uani 1 1 d .
H47A H 0.5072 0.3029 -0.4055 0.172 Uiso 1 1 calc R
H47B H 0.4182 0.2426 -0.3733 0.172 Uiso 1 1 calc R
H47C H 0.5491 0.2104 -0.3617 0.172 Uiso 1 1 calc R
C1S C 0.2100(10) 0.6101(10) 0.3234(4) 0.113(4) Uani 1 1 d .
H1SA H 0.2935 0.6066 0.3263 0.136 Uiso 1 1 calc R
H1SB H 0.1881 0.5675 0.3546 0.136 Uiso 1 1 calc R
Cl1 Cl 0.1563(5) 0.5564(4) 0.2662(2) 0.224(3) Uani 1 1 d .
Cl2 Cl 0.1706(4) 0.7443(3) 0.33206(17) 0.1574(14) 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
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'
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'
Br Br -0.2901 2.4595 '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'
Cl Cl 0.1484 0.1585 '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
N3 Mo1 N1 95.34(14) . .
N3 Mo1 Mo2 92.49(10) . .
N1 Mo1 Mo2 91.84(10) . .
N3 Mo1 Br2 159.95(10) . .
N1 Mo1 Br2 88.58(10) . .
Mo2 Mo1 Br2 107.06(2) . .
N3 Mo1 Br1 88.01(10) . .
N1 Mo1 Br1 163.03(10) . .
Mo2 Mo1 Br1 104.66(2) . .
Br2 Mo1 Br1 82.856(19) . .
N2 Mo2 N4 95.18(15) . .
N2 Mo2 Mo1 92.71(10) . .
N4 Mo2 Mo1 92.16(10) . .
N2 Mo2 Br2 159.26(10) . 3_655
N4 Mo2 Br2 90.41(11) . 3_655
Mo1 Mo2 Br2 107.05(2) . 3_655
N2 Mo2 Br1 85.99(11) . 3_655
N4 Mo2 Br1 163.14(10) . 3_655
Mo1 Mo2 Br1 104.59(2) . 3_655
Br2 Mo2 Br1 83.03(2) 3_655 3_655
Mo2 Br1 Mo1 88.00(2) 3_655 .
Mo2 Br2 Mo1 88.99(2) 3_655 .
C10 N1 C11 117.2(4) . .
C10 N1 Mo1 117.6(3) . .
C11 N1 Mo1 125.2(3) . .
C10 N2 C21 118.5(4) . .
C10 N2 Mo2 118.8(3) . .
C21 N2 Mo2 121.5(3) . .
C30 N3 C31 117.5(4) . .
C30 N3 Mo1 118.7(3) . .
C31 N3 Mo1 122.3(3) . .
C30 N4 C41 116.5(4) . .
C30 N4 Mo2 117.0(3) . .
C41 N4 Mo2 126.2(3) . .
C14 O1 C17 118.4(4) . .
C25 O2 C27 116.8(4) . .
C37 O3 C34 119.1(8) . .
C47 O4 C44 117.2(6) . .
N1 C10 N2 118.8(4) . .
C16 C11 C12 117.9(4) . .
C16 C11 N1 122.8(4) . .
C12 C11 N1 119.3(4) . .
C13 C12 C11 121.2(5) . .
C12 C13 C14 119.9(5) . .
O1 C14 C15 124.9(5) . .
O1 C14 C13 115.4(4) . .
C15 C14 C13 119.7(4) . .
C14 C15 C16 120.3(4) . .
C15 C16 C11 120.9(4) . .
C22 C21 C26 119.0(4) . .
C22 C21 N2 122.1(4) . .
C26 C21 N2 118.9(4) . .
C21 C22 C23 121.1(4) . .
C25 C23 C22 119.5(5) . .
C26 C24 C25 121.0(5) . .
O2 C25 C24 116.2(5) . .
O2 C25 C23 124.5(5) . .
C24 C25 C23 119.3(4) . .
C24 C26 C21 120.1(5) . .
N3 C30 N4 119.5(4) . .
C32 C31 C36 118.3(5) . .
C32 C31 N3 121.7(5) . .
C36 C31 N3 119.9(5) . .
C31 C32 C33 118.4(6) . .
C34 C33 C32 119.2(7) . .
C35 C34 C33 122.8(7) . .
C35 C34 O3 114.9(7) . .
C33 C34 O3 122.3(8) . .
C34 C35 C36 117.9(7) . .
C35 C36 C31 123.2(7) . .
C42 C41 C46 118.1(5) . .
C42 C41 N4 121.2(5) . .
C46 C41 N4 120.7(5) . .
C41 C42 C43 120.6(6) . .
C44 C43 C42 119.3(6) . .
C45 C44 C43 121.2(5) . .
C45 C44 O4 114.7(6) . .
C43 C44 O4 124.1(6) . .
C44 C45 C46 119.0(6) . .
C45 C46 C41 121.9(6) . .
Cl1 C1S Cl2 115.2(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 N3 2.074(4) .
Mo1 N1 2.115(4) .
Mo1 Mo2 2.1181(6) .
Mo1 Br2 2.6415(7) .
Mo1 Br1 2.6613(7) .
Mo2 N2 2.076(4) .
Mo2 N4 2.107(4) .
Mo2 Br2 2.6334(7) 3_655
Mo2 Br1 2.6604(6) 3_655
Br1 Mo2 2.6604(6) 3_655
Br2 Mo2 2.6334(7) 3_655
N1 C10 1.327(5) .
N1 C11 1.433(5) .
N2 C10 1.329(5) .
N2 C21 1.435(6) .
N3 C30 1.317(6) .
N3 C31 1.431(6) .
N4 C30 1.332(6) .
N4 C41 1.422(6) .
O1 C14 1.369(5) .
O1 C17 1.411(7) .
O2 C25 1.365(6) .
O2 C27 1.412(7) .
O3 C37 1.327(12) .
O3 C34 1.408(8) .
O4 C47 1.382(10) .
O4 C44 1.390(7) .
C11 C16 1.389(6) .
C11 C12 1.395(6) .
C12 C13 1.382(7) .
C13 C14 1.388(7) .
C14 C15 1.374(7) .
C15 C16 1.389(6) .
C21 C22 1.374(7) .
C21 C26 1.399(6) .
C22 C23 1.395(7) .
C23 C25 1.392(7) .
C24 C26 1.376(7) .
C24 C25 1.380(7) .
C31 C32 1.353(8) .
C31 C36 1.399(8) .
C32 C33 1.445(9) .
C33 C34 1.350(11) .
C34 C35 1.335(11) .
C35 C36 1.357(8) .
C41 C42 1.373(7) .
C41 C46 1.398(7) .
C42 C43 1.409(8) .
C43 C44 1.376(9) .
C44 C45 1.368(9) .
C45 C46 1.380(8) .
C1S Cl1 1.570(11) .
C1S Cl2 1.750(12) .
