#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:46:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178581 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/92/4069246.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_4069246
loop_
_publ_author_name
'Honzíček, Jan'
'Mukhopadhyay, Abhik'
'Santos-Silva, Teresa'
'Romão, Maria J.'
'Romão, Carlos C.'
_publ_section_title
;
 Ring-Functionalized Molybdenocene Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2871
_journal_paper_doi               10.1021/om9001022
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C13 H13 Mo N2 O4, B F4'
_chemical_formula_sum            'C13 H13 B F4 Mo N2 O4'
_chemical_formula_weight         444.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.4180(13)
_cell_length_b                   11.568(2)
_cell_length_c                   11.538(2)
_cell_measurement_reflns_used    8026
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.38
_cell_measurement_theta_min      2.51
_cell_volume                     848.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.891
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12579
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.9674
_exptl_absorpt_correction_T_min  0.8377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0273P)²+0.4821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                2239
_reflns_number_total             2416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9001022_si_002.cif
_cod_data_source_block           22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4069246
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mo1 Mo 0.64438(3) 0.7500 0.945961(15) 0.01652(6) Uani 1 2 d S
C1 C 0.2885(3) 0.81066(18) 0.88760(17) 0.0311(4) Uani 1 1 d .
C2 C 0.3667(3) 0.84959(16) 1.00136(16) 0.0269(4) Uani 1 1 d .
C3 C 0.4124(4) 0.7500 1.0735(2) 0.0241(5) Uani 1 2 d S
C4 C 0.4975(4) 0.7500 1.1992(2) 0.0401(7) Uani 1 2 d S
C5 C 0.6449(8) 0.8373(5) 1.3667(4) 0.0461(11) Uani 0.50 1 d P
H5A H 0.674(9) 0.923(6) 1.382(5) 0.070(18) Uiso 0.50 1 d P
H5B H 0.566(8) 0.795(4) 1.411(4) 0.048(14) Uiso 0.50 1 d P
H5C H 0.756(8) 0.800(4) 1.368(4) 0.051(16) Uiso 0.50 1 d P
C6 C 0.8375(2) 0.85350(15) 1.04593(14) 0.0232(3) Uani 1 1 d .
C7 C 0.7582(3) 0.58168(17) 0.73462(16) 0.0339(4) Uani 1 1 d .
C8 C 0.8019(5) 0.5137(2) 0.6350(2) 0.0649(8) Uani 1 1 d .
H8A H 0.7026 0.5332 0.5678 0.097 Uiso 1 1 calc R
H8B H 0.7901 0.4330 0.6522 0.097 Uiso 1 1 calc R
H8C H 0.9418 0.5300 0.6190 0.097 Uiso 1 1 calc R
O1 O 0.5345(2) 0.84685(14) 1.24817(12) 0.0412(3) Uani 1 1 d .
O2 O 0.9456(2) 0.91174(12) 1.10809(12) 0.0356(3) Uani 1 1 d .
N1 N 0.7254(2) 0.63524(13) 0.81181(12) 0.0262(3) Uani 1 1 d .
B1 B 0.2098(5) 0.7500 0.5630(3) 0.0317(6) Uani 1 2 d S
F1 F 0.3214(3) 0.65139(15) 0.59553(13) 0.0684(5) Uani 1 1 d .
F2 F 0.0317(4) 0.7500 0.6175(2) 0.0714(7) Uani 1 2 d S
F3 F 0.1535(3) 0.7500 0.44238(14) 0.0451(4) Uani 1 2 d S
H2 H 0.377(3) 0.920(2) 1.0278(18) 0.033(6) Uiso 1 1 d .
H1 H 0.255(3) 0.857(2) 0.8248(19) 0.036(6) Uiso 1 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'
B B 0.0013 0.0007 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 '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
C6 Mo1 C6 74.56(10) . 4_575
C6 Mo1 N1 81.50(6) . 4_575
C6 Mo1 N1 126.72(6) 4_575 4_575
C6 Mo1 N1 126.72(6) . .
C6 Mo1 N1 81.50(6) 4_575 .
N1 Mo1 N1 76.00(8) 4_575 .
C6 Mo1 C3 92.11(7) . .
C6 Mo1 C3 92.11(7) 4_575 .
N1 Mo1 C3 136.19(5) 4_575 .
N1 Mo1 C3 136.19(5) . .
C6 Mo1 C2 126.34(7) . 4_575
C6 Mo1 C2 88.97(7) 4_575 4_575
N1 Mo1 C2 141.75(6) 4_575 4_575
N1 Mo1 C2 99.48(6) . 4_575
C3 Mo1 C2 36.82(6) . 4_575
C6 Mo1 C2 88.97(7) . .
C6 Mo1 C2 126.34(7) 4_575 .
N1 Mo1 C2 99.48(6) 4_575 .
N1 Mo1 C2 141.75(6) . .
C3 Mo1 C2 36.82(6) . .
C2 Mo1 C2 60.53(10) 4_575 .
C6 Mo1 C1 146.99(7) . 4_575
C6 Mo1 C1 118.93(7) 4_575 4_575
N1 Mo1 C1 107.06(6) 4_575 4_575
N1 Mo1 C1 86.14(6) . 4_575
C3 Mo1 C1 59.26(8) . 4_575
C2 Mo1 C1 35.03(7) 4_575 4_575
C2 Mo1 C1 58.43(7) . 4_575
C6 Mo1 C1 118.93(7) . .
C6 Mo1 C1 146.99(7) 4_575 .
N1 Mo1 C1 86.14(6) 4_575 .
N1 Mo1 C1 107.06(6) . .
C3 Mo1 C1 59.26(8) . .
C2 Mo1 C1 58.43(7) 4_575 .
C2 Mo1 C1 35.03(7) . .
C1 Mo1 C1 34.06(10) 4_575 .
C1 C1 C2 108.59(11) 4_575 .
C1 C1 Mo1 72.97(5) 4_575 .
C2 C1 Mo1 68.24(9) . .
C1 C1 H1 126.3(14) 4_575 .
C2 C1 H1 124.9(14) . .
Mo1 C1 H1 121.0(14) . .
C1 C2 C3 107.63(17) . .
C1 C2 Mo1 76.73(10) . .
C3 C2 Mo1 69.59(11) . .
C1 C2 H2 128.6(14) . .
C3 C2 H2 123.6(14) . .
Mo1 C2 H2 123.2(14) . .
C2 C3 C2 107.5(2) 4_575 .
C2 C3 C4 126.22(11) 4_575 .
C2 C3 C4 126.21(11) . .
C2 C3 Mo1 73.59(11) 4_575 .
C2 C3 Mo1 73.59(11) . .
C4 C3 Mo1 117.18(16) . .
O1 C4 O1 125.1(3) 4_575 .
O1 C4 C3 117.42(13) 4_575 .
O1 C4 C3 117.41(13) . .
O1 C5 C5 94.4(3) . 4_575
O1 C5 H5A 98(3) . .
C5 C5 H5A 166(3) 4_575 .
O1 C5 H5B 110(3) . .
C5 C5 H5B 58(3) 4_575 .
H5A C5 H5B 121(4) . .
O1 C5 H5C 111(3) . .
C5 C5 H5C 59(3) 4_575 .
H5A C5 H5C 112(5) . .
H5B C5 H5C 104(4) . .
O2 C6 Mo1 176.94(15) . .
N1 C7 C8 179.4(2) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C4 O1 C5 113.0(3) . .
C7 N1 Mo1 173.86(15) . .
F1 B1 F1 112.5(3) . 4_575
F1 B1 F2 108.03(17) . .
F1 B1 F2 108.03(17) 4_575 .
F1 B1 F3 109.18(16) . .
F1 B1 F3 109.18(16) 4_575 .
F2 B1 F3 109.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C6 1.9766(17) .
Mo1 C6 1.9767(17) 4_575
Mo1 N1 2.1564(15) 4_575
Mo1 N1 2.1564(15) .
Mo1 C3 2.233(2) .
Mo1 C2 2.2858(18) 4_575
Mo1 C2 2.2858(17) .
Mo1 C1 2.3955(17) 4_575
Mo1 C1 2.3955(17) .
C1 C1 1.403(4) 4_575
C1 C2 1.413(3) .
C1 H1 0.90(2) .
C2 C3 1.428(2) .
C2 H2 0.87(2) .
C3 C2 1.428(2) 4_575
C3 C4 1.478(4) .
C4 O1 1.262(2) 4_575
C4 O1 1.262(2) .
C5 O1 1.455(5) .
C5 C5 2.019(12) 4_575
C5 H5A 1.02(6) .
C5 H5B 0.91(5) .
C5 H5C 0.83(5) .
C6 O2 1.146(2) .
C7 N1 1.128(2) .
C7 C8 1.452(3) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
B1 F1 1.372(2) .
B1 F1 1.372(2) 4_575
B1 F2 1.378(4) .
B1 F3 1.388(3) .
