#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:20:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178646 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075707.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_4075707
loop_
_publ_author_name
'Alvarez, Celedonio M.'
'Alvarez, M. Angeles'
'García, M. Esther'
'Ramos, Alberto'
'Ruiz, Miguel A.'
'Lanfranchi, Maurizio'
'Tiripicchio, Antonio'
_publ_section_title
;
 A Triply Bonded Dimolybdenum Hydride Complex with Acid, Base and Radical
 Activity
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              7
_journal_paper_doi               10.1021/om0491948
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C29 H42 Mo2 N O2 P'
_chemical_formula_weight         659.49
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2003-06-30T15:53:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                105.90(2)
_cell_angle_beta                 98.26(2)
_cell_angle_gamma                107.56(2)
_cell_formula_units_Z            2
_cell_length_a                   10.100(6)
_cell_length_b                   11.745(7)
_cell_length_c                   13.815(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1456.2(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4240
_diffrn_reflns_theta_full        24
_diffrn_reflns_theta_max         24
_diffrn_reflns_theta_min         3.1
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_refine_diff_density_max         2.116
_refine_diff_density_min         -1.996
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1563P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                3772
_reflns_number_total             4240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0491948si20041019_052159.cif
_cod_data_source_block           a60(compound_3)
_cod_original_cell_volume        1456.2(15)
_cod_database_code               4075707
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
C C 0.4670(6) 0.6434(5) 0.6305(4) 0.0304(12) Uani 1 d . . .
H H 0.4543 0.567 0.5732 0.036 Uiso 1 calc R . .
C1 C 0.5905(6) 0.8817(6) 0.8794(4) 0.0376(14) Uani 1 d . . .
C2 C 0.2240(7) 0.5886(6) 0.5592(4) 0.0457(14) Uani 1 d . . .
C3 C 0.6618(9) 0.5532(7) 0.7934(6) 0.0609(19) Uani 1 d . . .
H3 H 0.6016 0.4695 0.7585 0.073 Uiso 1 calc R . .
C4 C 0.7549(10) 0.6319(10) 0.7501(7) 0.072(3) Uani 1 d . . .
H4 H 0.7676 0.6105 0.683 0.086 Uiso 1 calc R . .
C5 C 0.8247(8) 0.7514(10) 0.8328(9) 0.083(3) Uani 1 d . . .
H5 H 0.8924 0.8232 0.8293 0.099 Uiso 1 calc R . .
C6 C 0.7729(9) 0.7403(9) 0.9192(7) 0.078(3) Uani 1 d . . .
H6 H 0.8002 0.804 0.9834 0.093 Uiso 1 calc R . .
C7 C 0.6755(8) 0.6207(7) 0.8943(6) 0.0576(19) Uani 1 d . . .
H7 H 0.626 0.59 0.9391 0.069 Uiso 1 calc R . .
C8 C 0.1744(9) 0.8236(8) 0.7634(7) 0.066(2) Uani 1 d . . .
H8 H 0.1327 0.7914 0.8106 0.079 Uiso 1 calc R . .
C9 C 0.2988(9) 0.9226(8) 0.7867(6) 0.0569(19) Uani 1 d . . .
H9 H 0.3574 0.9688 0.8531 0.068 Uiso 1 calc R . .
C10 C 0.3243(8) 0.9438(6) 0.7012(6) 0.0571(18) Uani 1 d . . .
H10 H 0.4046 1.007 0.6991 0.068 Uiso 1 calc R . .
C11 C 0.2178(9) 0.8612(8) 0.6159(5) 0.062(2) Uani 1 d . . .
H11 H 0.2109 0.8594 0.5476 0.075 Uiso 1 calc R . .
C12 C 0.1186(8) 0.7774(7) 0.6533(9) 0.086(3) Uani 1 d . . .
H12 H 0.0363 0.7083 0.6143 0.103 Uiso 1 calc R . .
C13 C 0.2546(5) 0.4491(5) 0.7517(4) 0.0309(11) Uani 1 d . . .
H13 H 0.2944 0.4222 0.6925 0.037 Uiso 1 calc R . .
C14 C 0.0917(6) 0.3960(5) 0.7070(4) 0.0392(13) Uani 1 d . . .
H14A H 0.045 0.4168 0.7625 0.047 Uiso 1 calc R . .
H14B H 0.0679 0.4355 0.6571 0.047 Uiso 1 calc R . .
C15 C 0.0361(7) 0.2529(6) 0.6541(5) 0.0539(18) Uani 1 d . . .
H15A H -0.0676 0.2219 0.6316 0.065 Uiso 1 calc R . .
H15B H 0.0728 0.2332 0.5928 0.065 Uiso 1 calc R . .
C16 C 0.0797(7) 0.1850(5) 0.7249(5) 0.0538(17) Uani 1 d . . .
H16A H 0.0494 0.0953 0.6858 0.065 Uiso 1 calc R . .
H16B H 0.0314 0.194 0.7808 0.065 Uiso 1 calc R . .
C17 C 0.2414(8) 0.2377(6) 0.7708(5) 0.0541(17) Uani 1 d . . .
H17A H 0.2647 0.1975 0.8202 0.065 Uiso 1 calc R . .
H17B H 0.2897 0.219 0.7159 0.065 Uiso 1 calc R . .
C18 C 0.2933(6) 0.3809(5) 0.8251(4) 0.0382(13) Uani 1 d . . .
H18A H 0.3965 0.4134 0.852 0.046 Uiso 1 calc R . .
H18B H 0.2506 0.3987 0.8834 0.046 Uiso 1 calc R . .
C19 C 0.2957(5) 0.6878(5) 0.9300(4) 0.0274(11) Uani 1 d . . .
H19 H 0.3145 0.778 0.9418 0.033 Uiso 1 calc R . .
C20 C 0.1382(6) 0.6301(5) 0.9330(4) 0.0326(12) Uani 1 d . . .
H20A H 0.0763 0.636 0.8755 0.039 Uiso 1 calc R . .
H20B H 0.1149 0.541 0.9247 0.039 Uiso 1 calc R . .
C21 C 0.1102(7) 0.6979(6) 1.0350(5) 0.0434(14) Uani 1 d . . .
H21A H 0.0107 0.6589 1.0348 0.052 Uiso 1 calc R . .
H21B H 0.1284 0.7861 1.042 0.052 Uiso 1 calc R . .
C22 C 0.2075(6) 0.6901(6) 1.1268(4) 0.0423(14) Uani 1 d . . .
H22A H 0.192 0.7364 1.1914 0.051 Uiso 1 calc R . .
H22B H 0.1839 0.6022 1.1229 0.051 Uiso 1 calc R . .
C23 C 0.3639(6) 0.7458(5) 1.1256(4) 0.0375(13) Uani 1 d . . .
H23A H 0.4236 0.7359 1.182 0.045 Uiso 1 calc R . .
H23B H 0.3896 0.8358 1.1372 0.045 Uiso 1 calc R . .
C24 C 0.3938(6) 0.6826(5) 1.0234(4) 0.0333(12) Uani 1 d . . .
H24A H 0.3793 0.5947 1.0157 0.04 Uiso 1 calc R . .
H24B H 0.493 0.7247 1.0246 0.04 Uiso 1 calc R . .
C25 C 0.6119(6) 0.8292(6) 0.5814(5) 0.0440(14) Uani 1 d . . .
C26 C 0.5084(11) 0.7912(12) 0.4764(7) 0.092(3) Uani 1 d . . .
H26A H 0.431 0.8211 0.4859 0.138 Uiso 1 calc R . .
H26B H 0.4709 0.7005 0.4452 0.138 Uiso 1 calc R . .
H26C H 0.5581 0.8282 0.4319 0.138 Uiso 1 calc R . .
C27 C 0.7339(10) 0.7786(11) 0.5634(8) 0.088(3) Uani 1 d . . .
H27A H 0.7997 0.8003 0.6288 0.132 Uiso 1 calc R . .
H27B H 0.7836 0.816 0.5191 0.132 Uiso 1 calc R . .
H27C H 0.6944 0.6881 0.5311 0.132 Uiso 1 calc R . .
C28 C 0.6715(10) 0.9714(7) 0.6353(8) 0.081(3) Uani 1 d . . .
H28A H 0.7392 0.9922 0.6996 0.122 Uiso 1 calc R . .
H28B H 0.5947 1.0005 0.6491 0.122 Uiso 1 calc R . .
H28C H 0.7185 1.0119 0.5914 0.122 Uiso 1 calc R . .
N N 0.5365(4) 0.7719(4) 0.6500(3) 0.0295(10) Uani 1 d . . .
O1 O 0.6116(6) 0.9779(4) 0.9410(4) 0.0685(14) Uani 1 d . . .
O2 O 0.1617(5) 0.5021(5) 0.4832(4) 0.0706(15) Uani 1 d . . .
P P 0.33977(13) 0.62565(11) 0.80334(9) 0.0234(3) Uani 1 d . . .
Mo1 Mo 0.58065(4) 0.71795(4) 0.78728(3) 0.0248(2) Uani 1 d . . .
Mo2 Mo 0.32601(4) 0.73632(4) 0.67878(3) 0.0242(2) Uani 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'
P P 0.1023 0.0942 '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
N C Mo1 74.5(3) . .
N C Mo2 72.7(3) . .
Mo1 C Mo2 86.3(2) . .
O1 C1 Mo1 171.3(5) . .
O2 C2 Mo2 176.6(6) . .
C7 C3 C4 109.0(8) . .
C7 C3 Mo1 74.3(4) . .
C4 C3 Mo1 72.0(4) . .
C3 C4 C5 105.0(7) . .
C3 C4 Mo1 72.4(4) . .
C5 C4 Mo1 72.3(5) . .
C6 C5 C4 107.7(7) . .
C6 C5 Mo1 73.7(4) . .
C4 C5 Mo1 71.8(4) . .
C7 C6 C5 108.9(8) . .
C7 C6 Mo1 73.3(4) . .
C5 C6 Mo1 71.8(4) . .
C6 C7 C3 109.4(8) . .
C6 C7 Mo1 73.1(4) . .
C3 C7 Mo1 71.9(4) . .
C9 C8 C12 107.8(7) . .
C9 C8 Mo2 75.3(4) . .
C12 C8 Mo2 69.4(4) . .
C10 C9 C8 109.8(7) . .
C10 C9 Mo2 72.9(4) . .
C8 C9 Mo2 71.7(4) . .
C9 C10 C11 111.5(7) . .
C9 C10 Mo2 75.2(4) . .
C11 C10 Mo2 71.8(4) . .
C10 C11 C12 105.9(7) . .
C10 C11 Mo2 74.5(4) . .
C12 C11 Mo2 69.8(4) . .
C8 C12 C11 104.9(6) . .
C8 C12 Mo2 74.8(4) . .
C11 C12 Mo2 74.0(4) . .
C18 C13 C14 109.5(4) . .
C18 C13 P 115.3(3) . .
C14 C13 P 115.6(4) . .
C15 C14 C13 111.3(5) . .
C16 C15 C14 112.5(5) . .
C15 C16 C17 111.8(5) . .
C18 C17 C16 110.2(5) . .
C17 C18 C13 111.9(5) . .
C24 C19 C20 109.1(4) . .
C24 C19 P 113.6(4) . .
C20 C19 P 116.0(3) . .
C21 C20 C19 111.7(4) . .
C20 C21 C22 110.1(5) . .
C23 C22 C21 110.3(4) . .
C22 C23 C24 112.3(4) . .
C23 C24 C19 111.7(5) . .
N C25 C28 107.4(5) . .
N C25 C26 109.8(5) . .
C28 C25 C26 111.7(7) . .
N C25 C27 109.2(5) . .
C28 C25 C27 110.7(7) . .
C26 C25 C27 108.1(8) . .
C N C25 126.4(5) . .
C N Mo2 69.4(3) . .
C25 N Mo2 135.4(3) . .
C N Mo1 67.8(3) . .
C25 N Mo1 140.5(3) . .
Mo2 N Mo1 83.16(14) . .
C13 P C19 109.4(2) . .
C13 P Mo1 117.33(18) . .
C19 P Mo1 118.65(17) . .
C13 P Mo2 116.77(17) . .
C19 P Mo2 118.08(17) . .
Mo1 P Mo2 72.90(4) . .
C1 Mo1 C 121.9(2) . .
C1 Mo1 N 91.5(2) . .
C Mo1 N 37.69(19) . .
C1 Mo1 C4 132.9(3) . .
C Mo1 C4 92.0(3) . .
N Mo1 C4 100.3(2) . .
C1 Mo1 C3 139.4(3) . .
C Mo1 C3 98.7(3) . .
N Mo1 C3 125.4(2) . .
C4 Mo1 C3 35.6(3) . .
C1 Mo1 C5 97.1(3) . .
C Mo1 C5 120.5(3) . .
N Mo1 C5 108.9(3) . .
C4 Mo1 C5 35.9(4) . .
C3 Mo1 C5 58.2(3) . .
C1 Mo1 C6 84.4(3) . .
C Mo1 C6 150.2(3) . .
N Mo1 C6 141.2(3) . .
C4 Mo1 C6 58.3(3) . .
C3 Mo1 C6 56.7(3) . .
C5 Mo1 C6 34.5(3) . .
C1 Mo1 C7 106.5(3) . .
C Mo1 C7 130.5(3) . .
N Mo1 C7 157.8(2) . .
C4 Mo1 C7 57.9(3) . .
C3 Mo1 C7 33.8(3) . .
C5 Mo1 C7 57.0(3) . .
C6 Mo1 C7 33.6(3) . .
C1 Mo1 P 88.76(18) . .
C Mo1 P 79.41(16) . .
N Mo1 P 100.40(11) . .
C4 Mo1 P 132.3(3) . .
C3 Mo1 P 99.0(2) . .
C5 Mo1 P 149.9(2) . .
C6 Mo1 P 118.0(3) . .
C7 Mo1 P 93.0(2) . .
C1 Mo1 Mo2 80.38(17) . .
C Mo1 Mo2 47.05(15) . .
N Mo1 Mo2 47.97(11) . .
C4 Mo1 Mo2 139.0(2) . .
C3 Mo1 Mo2 135.5(2) . .
C5 Mo1 Mo2 156.2(2) . .
C6 Mo1 Mo2 162.7(2) . .
C7 Mo1 Mo2 146.4(2) . .
P Mo1 Mo2 53.87(5) . .
C2 Mo2 C 70.3(2) . .
C2 Mo2 N 97.9(2) . .
C Mo2 N 37.89(19) . .
C2 Mo2 C12 84.0(3) . .
C Mo2 C12 153.1(3) . .
N Mo2 C12 145.7(3) . .
C2 Mo2 C11 93.0(3) . .
C Mo2 C11 134.7(2) . .
N Mo2 C11 109.7(3) . .
C12 Mo2 C11 36.2(3) . .
C2 Mo2 C8 113.3(3) . .
C Mo2 C8 167.5(2) . .
N Mo2 C8 146.1(3) . .
C12 Mo2 C8 35.8(3) . .
C11 Mo2 C8 57.8(3) . .
C2 Mo2 C10 126.2(3) . .
C Mo2 C10 133.7(2) . .
N Mo2 C10 96.4(2) . .
C12 Mo2 C10 57.4(3) . .
C11 Mo2 C10 33.6(3) . .
C8 Mo2 C10 54.9(3) . .
C2 Mo2 C9 141.2(3) . .
C Mo2 C9 147.5(3) . .
N Mo2 C9 113.1(2) . .
C12 Mo2 C9 57.2(3) . .
C11 Mo2 C9 55.6(3) . .
C8 Mo2 C9 33.0(3) . .
C10 Mo2 C9 31.9(3) . .
C2 Mo2 P 96.7(2) . .
C Mo2 P 78.69(15) . .
N Mo2 P 100.66(12) . .
C12 Mo2 P 113.2(3) . .
C11 Mo2 P 146.4(2) . .
C8 Mo2 P 88.90(17) . .
C10 Mo2 P 130.8(2) . .
C9 Mo2 P 99.6(2) . .
C2 Mo2 Mo1 111.5(2) . .
C Mo2 Mo1 46.66(15) . .
N Mo2 Mo1 48.87(12) . .
C12 Mo2 Mo1 159.2(3) . .
C11 Mo2 Mo1 148.1(2) . .
C8 Mo2 Mo1 123.5(2) . .
C10 Mo2 Mo1 116.82(18) . .
C9 Mo2 Mo1 106.45(18) . .
P Mo2 Mo1 53.23(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C N 1.388(7) .
C Mo1 2.101(6) .
C Mo2 2.115(6) .
C1 O1 1.149(7) .
C1 Mo1 1.959(6) .
C2 O2 1.171(7) .
C2 Mo2 1.914(6) .
C3 C7 1.366(11) .
C3 C4 1.426(12) .
C3 Mo1 2.335(7) .
C4 C5 1.437(14) .
C4 Mo1 2.330(7) .
C5 C6 1.392(13) .
C5 Mo1 2.337(8) .
C6 C7 1.365(11) .
C6 Mo1 2.361(7) .
C7 Mo1 2.363(6) .
C8 C9 1.353(12) .
C8 C12 1.429(12) .
C8 Mo2 2.359(6) .
C9 C10 1.316(11) .
C9 Mo2 2.404(7) .
C10 C11 1.366(10) .
C10 Mo2 2.377(6) .
C11 C12 1.439(13) .
C11 Mo2 2.343(6) .
C12 Mo2 2.288(7) .
C13 C18 1.530(8) .
C13 C14 1.535(8) .
C13 P 1.867(5) .
C14 C15 1.522(8) .
C15 C16 1.517(10) .
C16 C17 1.527(10) .
C17 C18 1.526(8) .
C19 C24 1.537(7) .
C19 C20 1.542(7) .
C19 P 1.874(5) .
C20 C21 1.528(8) .
C21 C22 1.530(9) .
C22 C23 1.522(8) .
C23 C24 1.523(8) .
C25 N 1.475(7) .
C25 C28 1.514(10) .
C25 C26 1.526(11) .
C25 C27 1.543(10) .
N Mo2 2.157(4) .
N Mo1 2.187(4) .
P Mo1 2.4163(19) .
P Mo2 2.4363(17) .
Mo1 Mo2 2.8831(15) .
