#------------------------------------------------------------------------------
#$Date: 2017-03-04 04:19:03 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193004 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/54/4345485.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_4345485
loop_
_publ_author_name
'Neary, Michelle C.'
'Parkin, Gerard'
_publ_section_title
;
 Reactivity of Cyclopentadienyl Molybdenum Compounds towards Formic Acid:
 Structural Characterization of CpMo(PMe3)(CO)2H, CpMo(PMe3)2(CO)H,
 [CpMo(μ-O)(μ-O2CH)]2, and [Cp*Mo(μ-O)(μ-O2CH)]2.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1511
_journal_page_last               1523
_journal_paper_doi               10.1021/acs.inorgchem.6b02606
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C10 H15 Mo O2 P'
_chemical_formula_sum            'C10 H15 Mo O2 P'
_chemical_formula_weight         294.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.671(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4275(17)
_cell_length_b                   12.152(2)
_cell_length_c                   12.291(2)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.81
_cell_measurement_theta_min      2.40
_cell_volume                     1217.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20362
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.928
_diffrn_reflns_theta_min         2.396
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6209
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.529
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         4360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0265
_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)+(0.0157P)²+1.4841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3944
_reflns_number_total             4360
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cpmoph_a.cif
_cod_data_source_block           cpmoph_a
_cod_database_code               4345485
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.643
_shelx_estimated_absorpt_t_max   0.798
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mo Mo 0.11576(2) 0.29144(2) 0.11673(2) 0.01897(4) Uani 1 1 d . .
H1 H 0.144(4) 0.262(2) 0.253(2) 0.047(8) Uiso 1 1 d . .
O1 O 0.4171(2) 0.39497(16) 0.05125(15) 0.0472(4) Uani 1 1 d . .
O2 O 0.1907(2) 0.48894(13) 0.28267(14) 0.0401(3) Uani 1 1 d . .
P1 P 0.32230(5) 0.15360(4) 0.18550(4) 0.02370(9) Uani 1 1 d . .
C1 C 0.3039(2) 0.35600(17) 0.07434(15) 0.0294(4) Uani 1 1 d . .
C2 C 0.1633(2) 0.41527(15) 0.22026(15) 0.0267(3) Uani 1 1 d . .
C3 C -0.1612(3) 0.2350(3) 0.0858(2) 0.0522(7) Uani 1 1 d . .
H3A H -0.2201 0.2203 0.1454 0.063 Uiso 1 1 calc R U
C4 C -0.1587(3) 0.3363(3) 0.0294(3) 0.0647(10) Uani 1 1 d . .
H4A H -0.2169 0.4053 0.0411 0.078 Uiso 1 1 calc R U
C5 C -0.0758(3) 0.3177(2) -0.0570(2) 0.0472(6) Uani 1 1 d . .
H5A H -0.0660 0.3709 -0.1170 0.057 Uiso 1 1 calc R U
C6 C -0.0303(3) 0.2070(2) -0.05070(17) 0.0358(4) Uani 1 1 d . .
H6A H 0.0196 0.1676 -0.1053 0.043 Uiso 1 1 calc R U
C7 C -0.0824(3) 0.1580(2) 0.03687(19) 0.0394(5) Uani 1 1 d . .
H7A H -0.0745 0.0777 0.0554 0.047 Uiso 1 1 calc R U
C11 C 0.5034(2) 0.19849(19) 0.29079(18) 0.0360(4) Uani 1 1 d . .
H11A H 0.5808 0.1371 0.3104 0.054 Uiso 1 1 calc R U
H11B H 0.4715 0.2232 0.3582 0.054 Uiso 1 1 calc R U
H11C H 0.5555 0.2594 0.2606 0.054 Uiso 1 1 calc R U
C12 C 0.2590(3) 0.03289(18) 0.2526(2) 0.0422(5) Uani 1 1 d . .
H12A H 0.3531 -0.0164 0.2785 0.063 Uiso 1 1 calc R U
H12B H 0.1717 -0.0059 0.1983 0.063 Uiso 1 1 calc R U
H12C H 0.2184 0.0562 0.3169 0.063 Uiso 1 1 calc R U
C13 C 0.4104(3) 0.0907(2) 0.0793(2) 0.0426(5) Uani 1 1 d . .
H13A H 0.4923 0.0358 0.1149 0.064 Uiso 1 1 calc R U
H13B H 0.4629 0.1476 0.0439 0.064 Uiso 1 1 calc R U
H13C H 0.3234 0.0550 0.0220 0.064 Uiso 1 1 calc R U
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'
O O 0.0106 0.0060 '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
C2 Mo C1 79.47(8)
C2 Mo C6 152.37(8)
C1 Mo C6 102.84(8)
C2 Mo C5 118.02(9)
C1 Mo C5 96.91(8)
C6 Mo C5 34.53(9)
C2 Mo C4 97.74(8)
C1 Mo C4 123.72(12)
C6 Mo C4 57.69(8)
C5 Mo C4 35.38(11)
C2 Mo C7 144.26(8)
C1 Mo C7 134.62(9)
C6 Mo C7 34.49(8)
C5 Mo C7 57.56(8)
C4 Mo C7 57.24(9)
C2 Mo C3 111.12(9)
C1 Mo C3 154.98(8)
C6 Mo C3 57.08(8)
C5 Mo C3 58.08(9)
C4 Mo C3 34.89(12)
C7 Mo C3 33.74(10)
C2 Mo P1 107.30(6)
C1 Mo P1 79.04(6)
C6 Mo P1 100.11(6)
C5 Mo P1 133.01(8)
C4 Mo P1 149.34(8)
C7 Mo P1 92.31(6)
C3 Mo P1 116.73(9)
C2 Mo H1 63.7(10)
C1 Mo H1 115.7(10)
C6 Mo H1 134.0(10)
C5 Mo H1 146.3(10)
C4 Mo H1 112.5(10)
C7 Mo H1 100.1(10)
C3 Mo H1 89.1(10)
P1 Mo H1 65.8(10)
C11 P1 C13 102.40(11)
C11 P1 C12 102.01(11)
C13 P1 C12 101.82(13)
C11 P1 Mo 116.30(8)
C13 P1 Mo 115.39(8)
C12 P1 Mo 116.68(8)
O1 C1 Mo 178.69(18)
O2 C2 Mo 179.35(18)
C7 C3 C4 108.1(2)
C7 C3 Mo 72.60(12)
C4 C3 Mo 71.96(14)
C7 C3 H3A 125.8
C4 C3 H3A 125.8
Mo C3 H3A 125.8
C3 C4 C5 107.2(2)
C3 C4 Mo 73.15(13)
C5 C4 Mo 72.13(12)
C3 C4 H4A 126.2
C5 C4 H4A 126.2
Mo C4 H4A 126.2
C6 C5 C4 106.9(2)
C6 C5 Mo 72.72(12)
C4 C5 Mo 72.48(13)
C6 C5 H5A 126.3
C4 C5 H5A 126.3
Mo C5 H5A 126.3
C5 C6 C7 108.6(2)
C5 C6 Mo 72.75(12)
C7 C6 Mo 73.03(12)
C5 C6 H6A 125.5
C7 C6 H6A 125.5
Mo C6 H6A 125.5
C3 C7 C6 109.2(2)
C3 C7 Mo 73.66(14)
C6 C7 Mo 72.48(12)
C3 C7 H7A 125.3
C6 C7 H7A 125.3
Mo C7 H7A 125.3
P1 C11 H11A 109.5
P1 C11 H11B 109.5
H11A C11 H11B 109.5
P1 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
P1 C12 H12A 109.5
P1 C12 H12B 109.5
H12A C12 H12B 109.5
P1 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
P1 C13 H13A 109.5
P1 C13 H13B 109.5
H13A C13 H13B 109.5
P1 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo C2 1.9458(19)
Mo C1 1.9542(19)
Mo C6 2.349(2)
Mo C5 2.350(2)
Mo C4 2.354(2)
Mo C7 2.356(2)
Mo C3 2.370(2)
Mo P1 2.4092(6)
Mo H1 1.67(3)
O1 C1 1.163(2)
O2 C2 1.163(2)
P1 C11 1.817(2)
P1 C13 1.825(2)
P1 C12 1.827(2)
C3 C7 1.371(4)
C3 C4 1.416(5)
C3 H3A 1.0000
C4 C5 1.429(4)
C4 H4A 1.0000
C5 C6 1.394(4)
C5 H5A 1.0000
C6 C7 1.395(3)
C6 H6A 1.0000
C7 H7A 1.0000
C11 H11A 0.9800
C11 H11B 0.9800
C11 H11C 0.9800
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
