#------------------------------------------------------------------------------
#$Date: 2018-06-26 18:43:21 +0300 (Tue, 26 Jun 2018) $
#$Revision: 208650 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/25/2242543.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_2242543
loop_
_publ_author_name
'Brown, Loren'
'Maron, Danny'
'Smith, Casey'
'Merola, Joseph'
_publ_section_title
;
 Crystal structure of the
 tetramethyl(phenethyl)cyclopentadienylmolybdenumtricarbonyl dimer
;
_journal_coeditor_code           PJ2053
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1017
_journal_page_last               1020
_journal_paper_doi               10.1107/S2056989018008885
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Mo2 (C17 H21)2 (C O)6]'
_chemical_formula_moiety         'C40 H42 Mo2 O6'
_chemical_formula_sum            'C40 H42 Mo2 O6'
_chemical_formula_weight         810.61
_chemical_name_systematic
Bis{tricarbonyl[η⁵-tetramethyl(phenethyl)cyclopentadienyl]molybdenum}(Mo---Mo)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.005(2)
_cell_angle_beta                 96.975(2)
_cell_angle_gamma                115.515(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2123(3)
_cell_length_b                   8.7728(3)
_cell_length_c                   13.4788(3)
_cell_measurement_reflns_used    13703
_cell_measurement_temperature    102.3(9)
_cell_measurement_theta_max      31.9860
_cell_measurement_theta_min      3.8330
_cell_volume                     867.24(5)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      102.3(9)
_diffrn_detector_area_resol_mean 8.0061
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku OD Xcalibur Eos Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27828
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.405
_diffrn_reflns_theta_min         3.824
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2018), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       irregular
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0280
_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)+(0.0220P)²+0.3543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                5362
_reflns_number_total             5873
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            pj2053sup1.cif
_cod_data_source_block           I
_cod_database_code               2242543
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Mo Mo1 0.93816(2) 0.48286(2) 0.61194(2) 0.00956(4) Uani d 1
O O1 0.78895(17) 0.71295(16) 0.70709(9) 0.0220(3) Uani d 1
O O2 0.56781(16) 0.37365(16) 0.46973(9) 0.0222(3) Uani d 1
O O3 1.24069(16) 0.85014(15) 0.60601(9) 0.0204(2) Uani d 1
C C1 0.8417(2) 0.6281(2) 0.66857(12) 0.0147(3) Uani d 1
C C2 0.7106(2) 0.4198(2) 0.51564(12) 0.0151(3) Uani d 1
C C3 1.1275(2) 0.7122(2) 0.59670(12) 0.0145(3) Uani d 1
C C4 0.8288(2) 0.30540(19) 0.73685(11) 0.0130(3) Uani d 1
C C5 1.0051(2) 0.43723(19) 0.77681(11) 0.0130(3) Uani d 1
C C6 1.1381(2) 0.41714(19) 0.72621(11) 0.0118(3) Uani d 1
C C7 1.0452(2) 0.27264(19) 0.65532(11) 0.0126(3) Uani d 1
C C8 0.8539(2) 0.20336(19) 0.66167(11) 0.0124(3) Uani d 1
C C9 1.0464(2) 0.5607(2) 0.86552(12) 0.0190(3) Uani d 1
H H9A 1.145490 0.669669 0.854880 0.028 Uiso calc 1
H H9B 1.083160 0.516547 0.926130 0.028 Uiso calc 1
H H9C 0.937299 0.576264 0.873419 0.028 Uiso calc 1
C C10 1.3404(2) 0.5136(2) 0.75498(12) 0.0177(3) Uani d 1
H H10A 1.401889 0.501161 0.699594 0.027 Uiso calc 1
H H10B 1.379416 0.468997 0.814706 0.027 Uiso calc 1
H H10C 1.372132 0.633737 0.769440 0.027 Uiso calc 1
C C11 1.1345(2) 0.1950(2) 0.59372(12) 0.0171(3) Uani d 1
H H11A 1.061270 0.153498 0.527506 0.026 Uiso calc 1
H H11B 1.143810 0.100409 0.627383 0.026 Uiso calc 1
H H11C 1.256743 0.280489 0.586017 0.026 Uiso calc 1
C C12 0.7090(2) 0.0385(2) 0.61166(13) 0.0189(3) Uani d 1
H H12A 0.596077 0.049941 0.592218 0.028 Uiso calc 1
H H12B 0.687155 -0.050467 0.658256 0.028 Uiso calc 1
H H12C 0.749102 0.008481 0.551819 0.028 Uiso calc 1
C C13 0.6516(2) 0.2734(2) 0.77284(12) 0.0170(3) Uani d 1
H H13A 0.552247 0.223631 0.715620 0.020 Uiso calc 1
H H13B 0.656572 0.383359 0.795769 0.020 Uiso calc 1
C C14 0.6044(2) 0.1545(2) 0.85895(13) 0.0202(3) Uani d 1
H H14A 0.580824 0.038789 0.834467 0.024 Uiso calc 1
H H14B 0.708000 0.195660 0.914158 0.024 Uiso calc 1
C C15 0.4371(2) 0.1511(2) 0.89656(12) 0.0163(3) Uani d 1
C C16 0.4522(2) 0.2522(2) 0.98076(13) 0.0224(4) Uani d 1
H H16 0.568229 0.314413 1.019772 0.027 Uiso calc 1
C C17 0.3000(2) 0.2640(2) 1.00913(14) 0.0246(4) Uani d 1
H H17 0.312472 0.332842 1.067395 0.029 Uiso calc 1
C C18 0.1313(2) 0.1754(2) 0.95232(14) 0.0216(3) Uani d 1
H H18 0.027715 0.185143 0.970506 0.026 Uiso calc 1
C C19 0.1133(2) 0.0722(2) 0.86855(13) 0.0213(3) Uani d 1
H H19 -0.003018 0.010151 0.829742 0.026 Uiso calc 1
C C20 0.2644(2) 0.0593(2) 0.84142(12) 0.0189(3) Uani d 1
H H20 0.250509 -0.012951 0.784518 0.023 Uiso calc 1
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 5 3 0.0576
5 3 -5 0.1547
5 -3 -3 0.1070
0 -5 1 0.1532
-1 0 -5 0.0903
0 -1 5 0.0638
2 1 5 0.1027
0 0 1 0.0270
0 0 -1 0.0561
1 -1 -5 0.0806
-2 0 5 0.0850
5 -4 5 0.0757
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
C1 Mo1 Mo1 2_766 123.14(5)
C1 Mo1 C2 . 79.57(6)
C1 Mo1 C3 . 77.69(6)
C1 Mo1 C4 . 87.41(6)
C1 Mo1 C5 . 84.52(6)
C1 Mo1 C6 . 115.39(6)
C1 Mo1 C7 . 142.19(6)
C1 Mo1 C8 . 120.77(6)
C2 Mo1 Mo1 2_766 74.11(5)
C2 Mo1 C4 . 101.17(6)
C2 Mo1 C5 . 135.42(6)
C2 Mo1 C6 . 152.82(6)
C2 Mo1 C7 . 120.20(6)
C2 Mo1 C8 . 94.42(6)
C3 Mo1 Mo1 2_766 68.01(5)
C3 Mo1 C2 . 112.68(6)
C3 Mo1 C4 . 139.37(6)
C3 Mo1 C5 . 103.97(6)
C3 Mo1 C6 . 93.26(6)
C3 Mo1 C7 . 116.21(6)
C3 Mo1 C8 . 150.35(6)
C4 Mo1 Mo1 2_766 146.34(4)
C4 Mo1 C5 . 36.34(5)
C4 Mo1 C6 . 59.42(5)
C4 Mo1 C7 . 58.65(5)
C4 Mo1 C8 . 35.55(5)
C5 Mo1 Mo1 2_766 145.99(4)
C5 Mo1 C6 . 35.42(5)
C5 Mo1 C7 . 58.51(5)
C5 Mo1 C8 . 59.37(5)
C6 Mo1 Mo1 2_766 110.63(4)
C6 Mo1 C7 . 34.79(5)
C6 Mo1 C8 . 58.58(5)
C7 Mo1 Mo1 2_766 94.24(4)
C8 Mo1 Mo1 2_766 110.83(4)
C8 Mo1 C7 . 34.83(5)
O1 C1 Mo1 . 176.27(14)
O2 C2 Mo1 . 171.42(14)
O3 C3 Mo1 . 167.87(14)
C5 C4 Mo1 . 71.87(8)
C5 C4 C13 . 125.92(14)
C8 C4 Mo1 . 74.90(9)
C8 C4 C5 . 107.90(13)
C8 C4 C13 . 126.06(14)
C13 C4 Mo1 . 122.25(10)
C4 C5 Mo1 . 71.79(8)
C4 C5 C9 . 126.16(14)
C6 C5 Mo1 . 74.82(8)
C6 C5 C4 . 108.20(13)
C6 C5 C9 . 125.19(14)
C9 C5 Mo1 . 125.37(11)
C5 C6 Mo1 . 69.76(8)
C5 C6 C7 . 107.84(13)
C5 C6 C10 . 125.02(14)
C7 C6 Mo1 . 74.13(8)
C7 C6 C10 . 126.43(14)
C10 C6 Mo1 . 129.10(11)
C6 C7 Mo1 . 71.08(8)
C6 C7 C8 . 108.39(13)
C6 C7 C11 . 125.66(14)
C8 C7 Mo1 . 71.18(8)
C8 C7 C11 . 125.60(14)
C11 C7 Mo1 . 128.87(10)
C4 C8 Mo1 . 69.55(8)
C4 C8 C7 . 107.68(13)
C4 C8 C12 . 125.14(14)
C7 C8 Mo1 . 73.99(8)
C7 C8 C12 . 126.49(14)
C12 C8 Mo1 . 129.29(10)
C5 C9 H9A . 109.5
C5 C9 H9B . 109.5
C5 C9 H9C . 109.5
H9A C9 H9B . 109.5
H9A C9 H9C . 109.5
H9B C9 H9C . 109.5
C6 C10 H10A . 109.5
C6 C10 H10B . 109.5
C6 C10 H10C . 109.5
H10A C10 H10B . 109.5
H10A C10 H10C . 109.5
H10B C10 H10C . 109.5
C7 C11 H11A . 109.5
C7 C11 H11B . 109.5
C7 C11 H11C . 109.5
H11A C11 H11B . 109.5
H11A C11 H11C . 109.5
H11B C11 H11C . 109.5
C8 C12 H12A . 109.5
C8 C12 H12B . 109.5
C8 C12 H12C . 109.5
H12A C12 H12B . 109.5
H12A C12 H12C . 109.5
H12B C12 H12C . 109.5
C4 C13 H13A . 108.6
C4 C13 H13B . 108.6
C4 C13 C14 . 114.48(13)
H13A C13 H13B . 107.6
C14 C13 H13A . 108.6
C14 C13 H13B . 108.6
C13 C14 H14A . 109.9
C13 C14 H14B . 109.9
H14A C14 H14B . 108.3
C15 C14 C13 . 108.93(13)
C15 C14 H14A . 109.9
C15 C14 H14B . 109.9
C16 C15 C14 . 121.01(15)
C16 C15 C20 . 118.16(15)
C20 C15 C14 . 120.50(15)
C15 C16 H16 . 119.4
C15 C16 C17 . 121.15(16)
C17 C16 H16 . 119.4
C16 C17 H17 . 120.1
C18 C17 C16 . 119.82(17)
C18 C17 H17 . 120.1
C17 C18 H18 . 120.1
C17 C18 C19 . 119.80(16)
C19 C18 H18 . 120.1
C18 C19 H19 . 119.9
C20 C19 C18 . 120.13(16)
C20 C19 H19 . 119.9
C15 C20 H20 . 119.5
C19 C20 C15 . 120.92(16)
C19 C20 H20 . 119.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mo1 Mo1 2_766 3.2773(3)
Mo1 C1 . 1.9536(16)
Mo1 C2 . 1.9943(16)
Mo1 C3 . 1.9764(16)
Mo1 C4 . 2.3065(15)
Mo1 C5 . 2.3076(14)
Mo1 C6 . 2.3737(14)
Mo1 C7 . 2.4135(14)
Mo1 C8 . 2.3767(15)
O1 C1 . 1.1532(19)
O2 C2 . 1.1526(19)
O3 C3 . 1.1579(19)
C4 C5 . 1.439(2)
C4 C8 . 1.431(2)
C4 C13 . 1.502(2)
C5 C6 . 1.425(2)
C5 C9 . 1.502(2)
C6 C7 . 1.432(2)
C6 C10 . 1.499(2)
C7 C8 . 1.434(2)
C7 C11 . 1.500(2)
C8 C12 . 1.500(2)
C9 H9A . 0.9800
C9 H9B . 0.9800
C9 H9C . 0.9800
C10 H10A . 0.9800
C10 H10B . 0.9800
C10 H10C . 0.9800
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 . 0.9900
C13 H13B . 0.9900
C13 C14 . 1.546(2)
C14 H14A . 0.9900
C14 H14B . 0.9900
C14 C15 . 1.510(2)
C15 C16 . 1.387(2)
C15 C20 . 1.397(2)
C16 H16 . 0.9500
C16 C17 . 1.395(3)
C17 H17 . 0.9500
C17 C18 . 1.380(3)
C18 H18 . 0.9500
C18 C19 . 1.388(3)
C19 H19 . 0.9500
C19 C20 . 1.384(2)
C20 H20 . 0.9500
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C10 H10A O2 2_766 0.98 2.54 3.277(2) 132
C12 H12B O1 1_545 0.98 2.62 3.432(2) 141
C12 H12C O3 2_766 0.98 2.47 3.127(2) 124
C20 H20 O3 1_445 0.95 2.65 3.579(2) 167

_cod_database_fobs_code 2242543
