#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:06:16 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301830 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/72/4077232.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_4077232
loop_
_publ_author_name
'Tamm, Matthias'
'Bannenberg, Thomas'
'Dressel, Bernd'
'Fröhlich, Roland'
'Kunz, Doris'
_publ_section_title
;
 Molybdenum Complexes with Sterically Demanding Cycloheptatrienyl Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              900
_journal_paper_doi               10.1021/om000830l
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C19 H31 B F4'
_chemical_formula_weight         346.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.57(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.223(5)
_cell_length_b                   10.936(3)
_cell_length_c                   18.195(6)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      21.15
_cell_volume                     1992.8(13)
_computing_cell_refinement       'Express (Nonius B.V., 1994)'
_computing_data_collection       'Express (Nonius B.V., 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_sigmaI/netI    0.1192
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3502
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         4.61
_diffrn_standards_decay_%        10.7
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.8952
_exptl_absorpt_correction_type   'empirical via \y scan data'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0887P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                1701
_reflns_number_total             3390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000830l.cif
_cod_data_source_block           han1222
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077232
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.0207(3) 0.1663(3) 0.84415(16) 0.0370(7) Uani 1 1 d .
C2 C -0.0576(3) 0.0690(3) 0.85809(16) 0.0385(7) Uani 1 1 d .
H2 H -0.0273 -0.0076 0.8451 0.046 Uiso 1 1 calc R
C3 C -0.1748(3) 0.0636(3) 0.88834(15) 0.0353(7) Uani 1 1 d .
C4 C -0.2318(3) 0.1617(3) 0.91850(16) 0.0401(8) Uani 1 1 d .
H4 H -0.3028 0.1396 0.9416 0.048 Uiso 1 1 calc R
C5 C -0.2047(3) 0.2863(3) 0.92129(15) 0.0376(7) Uani 1 1 d .
C6 C -0.1059(3) 0.3393(3) 0.88905(17) 0.0451(8) Uani 1 1 d .
H6 H -0.1049 0.4252 0.8903 0.054 Uiso 1 1 calc R
C7 C -0.0099(3) 0.2886(3) 0.85591(17) 0.0448(8) Uani 1 1 d .
H7 H 0.0450 0.3456 0.8380 0.054 Uiso 1 1 calc R
C8 C 0.1447(3) 0.1438(3) 0.81031(18) 0.0432(8) Uani 1 1 d .
C9 C 0.1839(4) 0.0096(3) 0.8104(3) 0.0871(15) Uani 1 1 d .
H9A H 0.2643 0.0012 0.7901 0.131 Uiso 1 1 calc R
H9B H 0.1121 -0.0367 0.7798 0.131 Uiso 1 1 calc R
H9C H 0.2004 -0.0214 0.8614 0.131 Uiso 1 1 calc R
C10 C 0.1138(4) 0.1906(4) 0.72865(18) 0.0694(11) Uani 1 1 d .
H10A H 0.0904 0.2766 0.7282 0.104 Uiso 1 1 calc R
H10B H 0.0396 0.1446 0.7000 0.104 Uiso 1 1 calc R
H10C H 0.1918 0.1800 0.7065 0.104 Uiso 1 1 calc R
C11 C 0.2630(3) 0.2148(4) 0.8543(2) 0.0682(11) Uani 1 1 d .
H11A H 0.2432 0.3017 0.8509 0.102 Uiso 1 1 calc R
H11B H 0.3415 0.1985 0.8335 0.102 Uiso 1 1 calc R
H11C H 0.2796 0.1896 0.9064 0.102 Uiso 1 1 calc R
C12 C -0.2362(3) -0.0642(3) 0.89041(16) 0.0422(8) Uani 1 1 d .
C13 C -0.1365(3) -0.1446(3) 0.94469(18) 0.0582(9) Uani 1 1 d .
H13A H -0.0524 -0.1480 0.9279 0.087 Uiso 1 1 calc R
H13B H -0.1725 -0.2266 0.9456 0.087 Uiso 1 1 calc R
H13C H -0.1222 -0.1099 0.9947 0.087 Uiso 1 1 calc R
C14 C -0.2630(3) -0.1182(3) 0.81070(17) 0.0512(9) Uani 1 1 d .
H14A H -0.3244 -0.0656 0.7773 0.077 Uiso 1 1 calc R
H14B H -0.3018 -0.1990 0.8114 0.077 Uiso 1 1 calc R
H14C H -0.1797 -0.1240 0.7931 0.077 Uiso 1 1 calc R
C15 C -0.3708(3) -0.0619(3) 0.9165(2) 0.0682(11) Uani 1 1 d .
H15A H -0.3574 -0.0300 0.9671 0.102 Uiso 1 1 calc R
H15B H -0.4064 -0.1443 0.9155 0.102 Uiso 1 1 calc R
H15C H -0.4333 -0.0101 0.8831 0.102 Uiso 1 1 calc R
C16 C -0.2932(3) 0.3724(3) 0.95663(18) 0.0506(9) Uani 1 1 d .
C17 C -0.3761(4) 0.3059(4) 1.0048(2) 0.0912(14) Uani 1 1 d .
H17A H -0.4378 0.2507 0.9736 0.137 Uiso 1 1 calc R
H17B H -0.4259 0.3651 1.0280 0.137 Uiso 1 1 calc R
H17C H -0.3176 0.2597 1.0435 0.137 Uiso 1 1 calc R
C18 C -0.3849(4) 0.4380(4) 0.8920(2) 0.0801(12) Uani 1 1 d .
H18A H -0.3314 0.4828 0.8627 0.120 Uiso 1 1 calc R
H18B H -0.4421 0.4945 0.9120 0.120 Uiso 1 1 calc R
H18C H -0.4395 0.3784 0.8603 0.120 Uiso 1 1 calc R
C19 C -0.2068(4) 0.4663(4) 1.0072(2) 0.0812(13) Uani 1 1 d .
H19A H -0.1414 0.4240 1.0446 0.122 Uiso 1 1 calc R
H19B H -0.2632 0.5164 1.0320 0.122 Uiso 1 1 calc R
H19C H -0.1612 0.5179 0.9770 0.122 Uiso 1 1 calc R
B B -0.0042(4) 0.6430(3) 0.7962(2) 0.0521(10) Uani 1 1 d .
F1 F -0.0561(2) 0.6781(3) 0.72435(14) 0.1087(9) Uani 1 1 d .
F2 F 0.0678(2) 0.73836(19) 0.83251(15) 0.0929(8) Uani 1 1 d .
F3 F -0.1060(2) 0.61341(17) 0.83244(14) 0.0828(7) Uani 1 1 d .
F4 F 0.0765(2) 0.54343(17) 0.79561(12) 0.0766(7) Uani 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 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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 C1 C7 123.5(3)
C2 C1 C8 120.2(3)
C7 C1 C8 116.2(3)
C1 C2 C3 131.9(3)
C4 C3 C2 125.3(3)
C4 C3 C12 119.2(2)
C2 C3 C12 115.4(3)
C3 C4 C5 132.6(3)
C4 C5 C6 123.3(3)
C4 C5 C16 119.2(3)
C6 C5 C16 117.4(3)
C7 C6 C5 131.5(3)
C6 C7 C1 131.0(3)
C9 C8 C11 108.1(3)
C9 C8 C1 113.1(3)
C11 C8 C1 109.9(3)
C9 C8 C10 109.0(3)
C11 C8 C10 108.9(3)
C1 C8 C10 107.8(2)
C3 C12 C14 108.8(2)
C3 C12 C15 112.7(3)
C14 C12 C15 107.1(3)
C3 C12 C13 108.3(2)
C14 C12 C13 110.7(3)
C15 C12 C13 109.1(3)
C17 C16 C18 109.9(3)
C17 C16 C5 113.1(3)
C18 C16 C5 106.8(3)
C17 C16 C19 107.1(3)
C18 C16 C19 109.7(3)
C5 C16 C19 110.2(3)
F1 B F4 109.7(3)
F1 B F2 108.4(3)
F4 B F2 110.1(3)
F1 B F3 109.8(3)
F4 B F3 109.4(3)
F2 B F3 109.4(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.385(4)
C1 C7 1.399(4)
C1 C8 1.537(4)
C2 C3 1.417(4)
C3 C4 1.385(4)
C3 C12 1.536(4)
C4 C5 1.389(4)
C5 C6 1.393(4)
C5 C16 1.533(4)
C6 C7 1.368(4)
C8 C9 1.521(4)
C8 C11 1.522(4)
C8 C10 1.543(4)
C12 C14 1.539(4)
C12 C15 1.543(4)
C12 C13 1.544(4)
C16 C17 1.521(4)
C16 C18 1.528(5)
C16 C19 1.535(5)
B F1 1.364(5)
B F4 1.367(4)
B F2 1.368(4)
B F3 1.377(4)
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
C7 C1 C2 C3 -3.2(5)
C8 C1 C2 C3 180.0(3)
C1 C2 C3 C4 -6.7(5)
C1 C2 C3 C12 176.6(3)
C2 C3 C4 C5 7.5(5)
C12 C3 C4 C5 -175.9(3)
C3 C4 C5 C6 1.5(5)
C3 C4 C5 C16 177.2(3)
C4 C5 C6 C7 -6.7(5)
C16 C5 C6 C7 177.6(3)
C5 C6 C7 C1 -0.5(6)
C2 C1 C7 C6 8.0(5)
C8 C1 C7 C6 -175.0(3)
C2 C1 C8 C9 -11.9(4)
C7 C1 C8 C9 171.0(3)
C2 C1 C8 C11 -132.8(3)
C7 C1 C8 C11 50.2(4)
C2 C1 C8 C10 108.6(3)
C7 C1 C8 C10 -68.4(4)
C4 C3 C12 C14 127.5(3)
C2 C3 C12 C14 -55.5(3)
C4 C3 C12 C15 8.8(4)
C2 C3 C12 C15 -174.2(3)
C4 C3 C12 C13 -112.0(3)
C2 C3 C12 C13 64.9(3)
C4 C5 C16 C17 16.8(4)
C6 C5 C16 C17 -167.3(3)
C4 C5 C16 C18 -104.2(3)
C6 C5 C16 C18 71.7(4)
C4 C5 C16 C19 136.7(3)
C6 C5 C16 C19 -47.4(4)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 15910450
