#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323436.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_4323436
loop_
_publ_author_name
'F. Albert Cotton'
'Günter Schmid'
_publ_section_title
;
 Mononuclear Molybdenum(IV) Complexes with Two Multiply Bonded Chalcogen
 Ligands in Trans Configuration and Chelating Biphosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2267
_journal_page_last               2278
_journal_paper_doi               10.1021/ic961071v
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'reac. of Mo(N2)2(dppee)2 and Se in toluene'
_chemical_formula_analytical     'not determined'
_chemical_formula_moiety         'C52 H44 Mo1 P4 Se2, C H2 Cl2'
_chemical_formula_structural
;
 Mo (Se)2 ( (C6 H5)2 P C H C H P (C6 H5)2 )2, C H2 Cl2
;
_chemical_formula_sum            'C53 H46 Cl2 Mo P4 Se2'
_chemical_formula_weight         1131.54
_chemical_name_common            'trans-Mo(Se)2₂(dppee)₂, CH2Cl2'
_chemical_name_systematic
;
trans-bis(cis-1,2-bis-(diphenylphosphino)ethylene-P,P')-di-selenido-
molybdenum (IV), dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.35(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.186(5)
_cell_length_b                   18.005(8)
_cell_length_c                   12.761(9)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      8.17
_cell_volume                     2410(2)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        MADNES
_computing_molecular_graphics    'ORTEP (Ulm, 1992)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Enraf Nonius FAST'
_diffrn_measurement_method       'ω rotation 0.2°'
_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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11257
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        'none observed'
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  'every image'
_diffrn_standards_number         'no standards, scaled on \b-lights'
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  'not measured'
_exptl_absorpt_correction_T_min  'not measured'
_exptl_absorpt_correction_type   'none applied'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not done'
_exptl_crystal_description       'block shaped crystal'
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       'none refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    'AFIX 43, common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_obs          0.0653
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0510P)²+25.3217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1684
_refine_ls_wR_factor_obs         0.1398
_reflns_number_observed          2571
_reflns_number_total             3579
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_3.cif
_cod_data_source_block           MoSe2dppee2_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (10 times).

'_geom_bond_publ_flag' value 'N'
changed to 'n' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (24
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (14 times).

'_geom_angle_publ_flag'
value 'N' changed to 'n' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(38 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not done' was changed to '?' -
the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+25.3217P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+25.3217P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2409.6(23)
_cod_database_code               4323436
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.0000 0.0000 0.0000 0.0190(3) Uani 1 d S .
Se1 Se -0.20056(8) 0.02577(5) -0.13599(7) 0.0295(3) Uani 1 d . .
P1 P 0.0969(2) 0.01188(12) -0.1499(2) 0.0219(5) Uani 1 d . .
P2 P 0.0451(2) 0.13647(12) 0.0098(2) 0.0222(5) Uani 1 d . .
C1 C 0.1055(8) 0.1111(5) -0.1790(7) 0.028(2) Uani 1 d . .
H1 H 0.1247(8) 0.1258(5) -0.2421(7) 0.044(8) Uiso 1 calc R .
C1A C 0.2593(8) -0.0186(5) -0.1319(6) 0.027(2) Uani 1 d . .
C1B C 0.3407(9) 0.0220(7) -0.1713(8) 0.046(3) Uani 1 d . .
H1B H 0.3144(9) 0.0689(7) -0.2036(8) 0.044(8) Uiso 1 calc R .
C1C C 0.4568(10) -0.0041(7) -0.1645(9) 0.056(3) Uani 1 d . .
H1C H 0.5111(10) 0.0253(7) -0.1894(9) 0.044(8) Uiso 1 calc R .
C1D C 0.4960(9) -0.0751(7) -0.1200(8) 0.047(3) Uani 1 d . .
H1D H 0.5747(9) -0.0946(7) -0.1180(8) 0.044(8) Uiso 1 calc R .
C1E C 0.4173(9) -0.1157(6) -0.0794(8) 0.044(3) Uani 1 d . .
H1E H 0.4432(9) -0.1628(6) -0.0478(8) 0.044(8) Uiso 1 calc R .
C1F C 0.2999(9) -0.0872(6) -0.0851(8) 0.038(2) Uani 1 d . .
H1F H 0.2472(9) -0.1152(6) -0.0565(8) 0.044(8) Uiso 1 calc R .
C1G C 0.0099(7) -0.0213(4) -0.2923(6) 0.020(2) Uani 1 d . .
C1H C 0.0428(8) -0.0873(5) -0.3322(7) 0.030(2) Uani 1 d . .
H1H H 0.1135(8) -0.1149(5) -0.2875(7) 0.044(8) Uiso 1 calc R .
C1I C -0.0293(9) -0.1120(6) -0.4381(7) 0.037(2) Uani 1 d . .
H1I H -0.0075(9) -0.1568(6) -0.4647(7) 0.044(8) Uiso 1 calc R .
C1K C -0.1316(9) -0.0722(6) -0.5045(7) 0.038(2) Uani 1 d . .
H1K H -0.1799(9) -0.0898(6) -0.5760(7) 0.044(8) Uiso 1 calc R .
C1L C -0.1641(9) -0.0057(6) -0.4664(7) 0.037(2) Uani 1 d . .
H1L H -0.2336(9) 0.0222(6) -0.5124(7) 0.044(8) Uiso 1 calc R .
C1M C -0.0941(8) 0.0191(5) -0.3609(7) 0.028(2) Uani 1 d . .
H1M H -0.1166(8) 0.0639(5) -0.3348(7) 0.044(8) Uiso 1 calc R .
C2 C 0.0851(8) 0.1630(5) -0.1122(7) 0.026(2) Uani 1 d . .
H2 H 0.0913(8) 0.2135(5) -0.1282(7) 0.045(8) Uiso 1 calc R .
C2A C 0.1764(7) 0.1784(5) 0.1247(6) 0.023(2) Uani 1 d . .
C2B C 0.2032(9) 0.1541(6) 0.2329(7) 0.036(2) Uani 1 d . .
H2B H 0.1557(9) 0.1147(6) 0.2470(7) 0.045(8) Uiso 1 calc R .
C2C C 0.2975(9) 0.1863(6) 0.3202(8) 0.042(2) Uani 1 d . .
H2C H 0.3136(9) 0.1689(6) 0.3933(8) 0.045(8) Uiso 1 calc R .
C2D C 0.3695(9) 0.2443(6) 0.3022(9) 0.047(3) Uani 1 d . .
H2D H 0.4341(9) 0.2663(6) 0.3625(9) 0.045(8) Uiso 1 calc R .
C2E C 0.3453(10) 0.2690(6) 0.1955(10) 0.051(3) Uani 1 d . .
H2E H 0.3940(10) 0.3081(6) 0.1822(10) 0.045(8) Uiso 1 calc R .
C2F C 0.2493(8) 0.2369(5) 0.1064(7) 0.035(2) Uani 1 d . .
H2F H 0.2332(8) 0.2545(5) 0.0335(7) 0.045(8) Uiso 1 calc R .
C2G C -0.0813(8) 0.2036(5) -0.0047(6) 0.026(2) Uani 1 d . .
C2H C -0.1714(9) 0.2170(5) -0.1109(8) 0.038(2) Uani 1 d . .
H2H H -0.1622(9) 0.1927(5) -0.1728(8) 0.045(8) Uiso 1 calc R .
C2I C -0.2725(10) 0.2644(6) -0.1278(9) 0.048(3) Uani 1 d . .
H2I H -0.3312(10) 0.2725(6) -0.2002(9) 0.045(8) Uiso 1 calc R .
C2K C -0.2866(9) 0.3002(5) -0.0366(9) 0.042(2) Uani 1 d . .
H2K H -0.3541(9) 0.3339(5) -0.0474(9) 0.045(8) Uiso 1 calc R .
C2L C -0.2029(9) 0.2868(5) 0.0694(8) 0.037(2) Uani 1 d . .
H2L H -0.2148(9) 0.3098(5) 0.1311(8) 0.045(8) Uiso 1 calc R .
C2M C -0.1011(8) 0.2396(5) 0.0850(7) 0.030(2) Uani 1 d . .
H2M H -0.0435(8) 0.2315(5) 0.1578(7) 0.045(8) Uiso 1 calc R .
C3 C 0.4585(19) 0.0114(12) 0.4151(16) 0.042(5) Uiso 0.50 d P .
Cl3A Cl 0.4746(7) -0.0847(5) 0.4075(7) 0.077(2) Uiso 0.50 d P .
Cl3B Cl 0.5106(6) 0.0512(5) 0.5477(6) 0.070(2) Uiso 0.50 d P .
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
_geom_angle_publ_flag
Se1 Mo1 P1 88.56(7) . . y
Se1 Mo1 P1 91.45(7) . 3 y
Se1 Mo1 P2 88.12(6) . . y
Se1 Mo1 P2 91.88(6) . 3 y
P2 Mo1 P1 79.71(7) . . y
P2 Mo1 P1 100.29(7) . 3 y
C1 P1 C1A 101.4(4) . . y
C1 P1 C1G 99.4(4) . . y
C1A P1 C1G 100.8(4) . . y
Mo1 P1 C1 107.7(3) . . n
Mo1 P1 C1A 123.3(3) . . n
Mo1 P1 C1G 120.3(2) . . n
P1 C1 C2 121.3(6) . . y
P1 C1A C1B 122.8(8) . . n
P1 C1A C1F 119.0(7) . . n
P1 C1G C1H 121.5(6) . . n
P1 C1G C1M 119.4(6) . . n
C1F C1A C1B 118.0(9) . . n
C1A C1B C1C 121.8(11) . . n
C1B C1C C1D 119.9(9) . . n
C1C C1D C1E 119.0(9) . . n
C1D C1E C1F 120.1(11) . . n
C1E C1F C1A 121.1(9) . . n
C1M C1G C1H 119.0(7) . . n
C1G C1H C1I 119.6(8) . . n
C1H C1I C1K 120.9(9) . . n
C1I C1K C1L 120.0(8) . . n
C1K C1L C1M 119.6(9) . . n
C1L C1M C1G 120.8(9) . . n
C2 P2 C2A 102.0(4) . . y
C2 P2 C2G 98.7(4) . . y
C2A P2 C2G 100.7(4) . . y
Mo1 P2 C2 108.6(3) . . n
Mo1 P2 C2A 122.3(3) . . n
Mo1 P2 C2G 120.7(3) . . n
P2 C2 C1 120.5(7) . . y
P2 C2A C2B 120.3(7) . . n
P2 C2A C2F 121.7(6) . . n
P2 C2G C2H 119.0(6) . . n
P2 C2G C2M 124.3(6) . . n
C2F C2A C2B 118.0(8) . . n
C2A C2B C2C 121.2(10) . . n
C2B C2C C2D 120.8(10) . . n
C2C C2D C2E 119.0(9) . . n
C2D C2E C2F 120.5(10) . . n
C2E C2F C2A 120.4(8) . . n
C2M C2G C2H 116.5(8) . . n
C2G C2H C2I 122.4(9) . . n
C2H C2I C2K 119.0(9) . . n
C2I C2K C2L 120.5(9) . . n
C2K C2L C2M 119.8(8) . . n
C2L C2M C2G 121.7(8) . . n
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 Se1 2.356(2) . y
Mo1 P1 2.514(2) . y
Mo1 P2 2.503(2) . y
P1 C1 1.834(9) . y
P1 C1A 1.835(9) . y
P1 C1G 1.837(8) . y
P2 C2 1.826(8) . y
P2 C2A 1.838(8) . y
P2 C2G 1.820(9) . y
C1 C2 1.337(12) . y
C1A C1B 1.391(13) . n
C1A C1F 1.378(13) . n
C1B C1C 1.355(14) . n
C1C C1D 1.41(2) . n
C1D C1E 1.376(15) . n
C1E C1F 1.388(13) . n
C1G C1H 1.391(11) . n
C1G C1M 1.392(12) . n
C1H C1I 1.384(12) . n
C1I C1K 1.367(14) . n
C1K C1L 1.387(14) . n
C1L C1M 1.376(12) . n
C2A C2B 1.378(12) . n
C2A C2F 1.401(12) . n
C2B C2C 1.369(13) . n
C2C C2D 1.385(15) . n
C2D C2E 1.368(15) . n
C2E C2F 1.389(13) . n
C2G C2H 1.400(12) . n
C2G C2M 1.399(12) . n
C2H C2I 1.373(14) . n
C2I C2K 1.387(14) . n
C2K C2L 1.372(14) . n
C2L C2M 1.379(13) . n
