#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010393.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2010393
loop_
_publ_author_name
'Pombeiro, A.J.L.'
'Hills, A.'
'Hughes, D.L.'
'Richards, R.L.'
_publ_section_title
;
 [MoH₄(dppe)₂].thf (dppe = Ph₂PCH₂CH₂PPh₂; thf =
 Tetrahydrofuran)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              23
_journal_page_last               26
_journal_paper_doi               10.1107/S0108270194007559
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C52 H52 Mo P , C4 H8 O'
_chemical_formula_sum            'C56 H60 Mo O P4'
_chemical_formula_weight         968.9
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.
_cell_angle_beta                 104.638(7)
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   15.7430(10)
_cell_length_b                   10.3000(10)
_cell_length_c                   15.8300(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     2483.6(3)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω-θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.005
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4573
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        'steady decrease to 86.3% of starting values'
_diffrn_standards_interval_time  167
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.42
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown-yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       'rectangular prisms'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.13
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4373
_refine_ls_R_factor_obs          0.032
_refine_ls_shift/esd_max         '1.33 (in disordered solvent atoms)'
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.040
_reflns_number_observed          3882
_reflns_number_total             4373
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            mu1119.cif
_cod_data_source_block           mu1119_structure_1_of_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F)' 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^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2483.5
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2010393
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,-y,1/2+z
-x,-y,-z
1/2-x,y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Mo .2500 .14111(2) 0.25 .03250(10) 1.0
C(11a) .00860(10) .1101(2) .2120(1) .0448(7) 1.0
C(12a) -.0432(2) .1792(3) .2540(2) .0640(10) 1.0
C(13a) -.1076(2) .1171(3) .2862(2) .0810(10) 1.0
C(14a) -.1192(2) -.0144(4) .2753(2) .0820(10) 1.0
C(15a) -.0684(2) -.0837(3) .2342(2) .0830(10) 1.0
C(16a) -.0038(2) -.0226(3) .2033(2) .0640(10) 1.0
C(11b) .05850(10) .3547(2) .1555(1) .0430(7) 1.0
C(12b) -.0237(2) .3805(2) .1022(2) .0549(9) 1.0
C(13b) -.0534(2) .5065(3) .0849(2) .0660(10) 1.0
C(14b) -.0013(2) .6081(3) .1199(2) .0700(10) 1.0
C(15b) .0814(2) .5858(3) .1709(2) .0750(10) 1.0
C(16b) .1111(2) .4598(2) .1889(2) .0606(9) 1.0
P(1) .09885(3) .18650(5) .17609(3) .0366(2) 1.0
C(1) .08050(10) .1269(2) .0625(1) .0450(7) 1.0
C(2) .15920(10) .1644(2) .0284(1) .0457(8) 1.0
P(2) .26071(3) .10064(5) .10217(3) .0368(2) 1.0
C(21a) .26400(10) -.0670(2) .0627(1) .0424(7) 1.0
C(22a) .2966(2) -.1646(2) .1208(2) .0760(10) 1.0
C(23a) .3018(3) -.2909(3) .0935(2) .097(2) 1.0
C(24a) .2733(2) -.3225(3) .0077(2) .0740(10) 1.0
C(25a) .2410(2) -.2283(3) -.0514(2) .0700(10) 1.0
C(26a) .2360(2) -.1008(3) -.0245(2) .0595(9) 1.0
C(21b) .3459(2) .1802(2) .0593(1) .0464(8) 1.0
C(22b) .3976(2) .1169(3) .0152(2) .0770(10) 1.0
C(23b) .4640(2) .1801(4) -.0108(3) .095(2) 1.0
C(24b) .4792(2) .3063(4) .0055(3) .099(2) 1.0
C(25b) .4294(3) .3732(3) .0511(3) .115(2) 1.0
C(26b) .3632(2) .3107(3) .0765(2) .088(2) 1.0
H(3) .2597(12) .276(2) .1954(12) .044(5) 1.0
H(4) .1871(14) .007(2) .2220(13) .057(7) 1.0
O(50) -.2500 .4228(14) 0.25 .146(4) 0.4
C(51) -.1817(18) .507(3) .3132(15) .176(9) 0.4
C(52) -.219(2) .620(3) .3281(15) .175(9) 0.4
C(53) -.1911(17) .481(3) .2361(22) .184(9) 0.4
C(54) -.1633(16) .578(3) .2770(24) .193(9) 0.4
O(55) -.2500 .689(2) 0.25 .215(8) 0.4
C(61) -.235(5) .647(4) .1902(33) .149(13) 0.2
C(62) -.252(3) .499(3) .1846(20) .135(9) 0.2
C(63) -.190(4) .634(4) .2897(33) .153(13) 0.2
C(64) -.200(4) .611(6) .2084(41) .144(19) 0.2
C(65) -.1883(18) .461(3) .2816(28) .102(7) 0.2
H(12a) -.0350 .2732 .2615 .081(9) 1.0
H(13a) -.1438 .1671 .3165 .083(9) 1.0
H(14a) -.1645 -.0580 .2974 .114(12) 1.0
H(15a) -.0777 -.1774 .2262 .112(12) 1.0
H(16a) .0335 -.0743 .1751 .077(9) 1.0
H(12b) -.0618 .3082 .0759 .070(8) 1.0
H(13b) -.1123 .5228 .0476 .099(10) 1.0
H(14b) -.0228 .6973 .1085 .076(8) 1.0
H(15b) .1196 .6591 .1948 .127(13) 1.0
H(16b) .1703 .4449 .2258 .073(8) 1.0
H(1)a .0272 .1663 .0259 .054(7) 1.0
H(1)b .0742 .0322 .0614 .039(5) 1.0
H(2)a .1523 .1280 -.0301 .059(7) 1.0
H(2)b .1628 .2592 .0257 .048(6) 1.0
H(22a) .3165 -.1443 .1832 .103(11) 1.0
H(23a) .3262 -.3385 .1364 .125(14) 1.0
H(24a) .2761 -.4127 -.0112 .116(12) 1.0
H(25a) .2214 -.2503 -.1136 .099(10) 1.0
H(26a) .2120 -.0337 -.0679 .073(8) 1.0
H(22b) .3874 .0244 .0020 .108(11) 1.0
H(23b) .5000 .1319 -.0424 .111(12) 1.0
H(24b) .5259 .3507 -.0140 .141(15) 1.0
H(25b) .4408 .4653 .0648 .135(14) 1.0
H(26b) .3274 .3594 .1080 .103(11) 1.0
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P(1) Mo P(1) 4 157.70(2) yes
P(1) Mo P(2) . 82.30(2) yes
P(1) Mo P(2) 4 101.56(2) yes
P(1) Mo H(3) . 78.2(7) yes
P(1) Mo H(3) 4 83.2(7) yes
P(1) Mo H(4) . 65.9(7) yes
P(1) Mo H(4) 4 136.4(7) yes
P(2) Mo P(2) 4 160.20(2) yes
P(2) Mo H(3) . 66.7(7) yes
P(2) Mo H(3) 4 133.1(7) yes
P(2) Mo H(4) . 77.6(7) yes
P(2) Mo H(4) 4 86.2(7) yes
H(3) Mo H(3) 4 66.8(9) yes
H(3) Mo H(4) . 132.1(10) yes
H(3) Mo H(4) 4 133.9(9) yes
H(4) Mo H(4) 4 70.6(10) yes
Mo P(1) C(11a) . 120.80(10) yes
Mo P(1) C(11b) . 121.30(10) yes
Mo P(1) C(1) . 107.40(10) yes
C(11a) P(1) C(11b) . 101.50(10) yes
C(11a) P(1) C(1) . 102.40(10) yes
C(11b) P(1) C(1) . 100.20(10) yes
Mo P(2) C(21a) . 120.20(10) yes
Mo P(2) C(21b) . 120.90(10) yes
Mo P(2) C(2) . 106.80(10) yes
C(21a) P(2) C(21b) . 101.90(10) yes
C(2) P(2) C(21a) . 102.30(10) yes
C(2) P(2) C(21b) . 101.80(10) yes
C(16b) C(11b) P(1) . 121.4(2) no
C(11b) C(12b) C(13b) . 121.3(2) no
C(12b) C(13b) C(14b) . 120.2(2) no
C(13b) C(14b) C(15b) . 119.8(2) no
C(14b) C(15b) C(16b) . 120.1(3) no
C(11b) C(16b) C(15b) . 121.1(2) no
P(1) C(1) C(2) . 108.60(10) no
P(2) C(21b) C(26b) . 119.0(2) no
C(21b) C(22b) C(23b) . 121.5(3) no
C(22b) C(23b) C(24b) . 120.9(3) no
C(23b) C(24b) C(25b) . 119.4(3) no
C(24b) C(25b) C(26b) . 119.7(3) no
C(21b) C(26b) C(25b) . 121.7(3) no
C(1) C(2) P(2) . 109.80(10) no
C(12a) C(11a) C(16a) . 118.3(2) no
C(12a) C(11a) P(1) . 121.9(2) no
C(16a) C(11a) P(1) . 119.6(2) no
C(11a) C(12a) C(13a) . 120.8(3) no
C(12a) C(13a) C(14a) . 119.5(3) no
C(13a) C(14a) C(15a) . 120.3(3) no
C(14a) C(15a) C(16a) . 120.3(3) no
C(11a) C(16a) C(15a) . 120.8(3) no
C(12b) C(11b) C(16b) . 117.4(2) no
C(12b) C(11b) P(1) . 121.1(2) no
C(22a) C(21a) C(26a) . 117.1(2) no
P(2) C(21a) C(22a) . 119.9(2) no
P(2) C(21a) C(26a) . 123.0(2) no
C(21a) C(22a) C(23a) . 121.5(3) no
C(22a) C(23a) C(24a) . 120.6(3) no
C(23a) C(24a) C(25a) . 119.4(3) no
C(24a) C(25a) C(26a) . 120.4(2) no
C(21a) C(26a) C(25a) . 121.0(2) no
C(22b) C(21b) C(26b) . 116.8(2) no
P(2) C(21b) C(22b) . 124.1(2) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo P(1) . . 2.4170(10) yes
Mo P(2) . . 2.4240(10) yes
Mo H(3) . . 1.66(2) yes
Mo H(4) . . 1.69(2) yes
P(1) C(1) . . 1.852(2) yes
P(1) C(11a) . . 1.835(2) yes
P(1) C(11b) . . 1.845(2) yes
P(2) C(2) . . 1.845(2) yes
P(2) C(21a) . . 1.841(2) yes
P(2) C(21b) . . 1.841(2) yes
C(11a) C(12a) . . 1.374(3) no
C(11a) C(16a) . . 1.382(3) no
C(12a) C(13a) . . 1.399(4) no
C(13a) C(14a) . . 1.371(4) no
C(14a) C(15a) . . 1.355(4) no
C(15a) C(16a) . . 1.386(4) no
C(11b) C(12b) . . 1.381(3) no
C(11b) C(16b) . . 1.384(3) no
C(12b) C(13b) . . 1.383(3) no
C(13b) C(14b) . . 1.359(4) no
C(14b) C(15b) . . 1.367(4) no
C(15b) C(16b) . . 1.384(3) no
C(1) C(2) . . 1.521(3) no
C(21a) C(22a) . . 1.371(3) no
C(21a) C(26a) . . 1.384(3) no
C(22a) C(23a) . . 1.380(4) no
C(23a) C(24a) . . 1.359(4) no
C(24a) C(25a) . . 1.355(4) no
C(25a) C(26a) . . 1.389(4) no
C(21b) C(22b) . . 1.364(4) no
C(21b) C(26b) . . 1.385(4) no
C(22b) C(23b) . . 1.380(4) no
C(23b) C(24b) . . 1.335(5) no
C(24b) C(25b) . . 1.377(5) no
C(25b) C(26b) . . 1.368(4) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
P(1) C(1) C(2) P(2) 55.7(2) yes
