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#$Date: 2016-03-23 22:51:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179493 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/90/4339018.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_4339018
loop_
_publ_author_name
'Kim, Do Young'
'Yang, Yu'
'Abelson, John R.'
'Girolami, Gregory S.'
_publ_section_title
;
 Volatile magnesium octahydrotriborate complexes as potential CVD
 precursors to MgB2. Synthesis and characterization of Mg(B3H8)2 and its
 etherates.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9060
_journal_page_last               9066
_journal_paper_doi               10.1021/ic701037t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C14 H18 Mg O'
_chemical_formula_sum            'C14 H18 Mg O'
_chemical_formula_weight         226.59
_chemical_name_common            bis(cyclopentadienyl)(tetrahydrofuran)magnesium
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 116.721(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.414(16)
_cell_length_b                   9.855(12)
_cell_length_c                   11.556(14)
_cell_measurement_temperature    193(2)
_cell_volume                     1263(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4047
_diffrn_reflns_av_sigmaI/netI    0.2416
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6392
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1161
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1944
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0530P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.2045
_reflns_number_gt                487
_reflns_number_total             1161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701037t-file004.cif
_cod_data_source_block           f01zface
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4339018
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Mg1 Mg 0.0000 0.1431(2) 0.2500 0.0344(8) Uani 1 2 d S
C1 C 0.2155(5) 0.1733(6) 0.3144(5) 0.0446(15) Uani 1 1 d D
H1 H 0.245(5) 0.264(3) 0.334(4) 0.054 Uiso 1 1 d D
C2 C 0.2058(5) 0.0692(6) 0.3902(4) 0.0446(15) Uani 1 1 d D
H2 H 0.242(4) 0.091(5) 0.480(3) 0.054 Uiso 1 1 d D
C3 C 0.1494(5) -0.0440(6) 0.3115(4) 0.0444(16) Uani 1 1 d D
H3 H 0.133(5) -0.131(3) 0.337(4) 0.053 Uiso 1 1 d D
C4 C 0.1207(5) -0.0057(7) 0.1826(4) 0.0455(16) Uani 1 1 d D
H4 H 0.080(4) -0.064(4) 0.109(3) 0.055 Uiso 1 1 d D
C5 C 0.1622(5) 0.1280(6) 0.1832(5) 0.0455(16) Uani 1 1 d D
H5 H 0.167(5) 0.183(4) 0.117(4) 0.055 Uiso 1 1 d D
O1 O 0.0000 0.3554(5) 0.2500 0.0392(14) Uani 1 2 d S
C6 C 0.0267(5) 0.4448(6) 0.1627(5) 0.0422(16) Uani 1 1 d D
H6A H -0.023(4) 0.400(4) 0.076(3) 0.051 Uiso 1 1 d D
H6B H 0.115(2) 0.447(5) 0.182(4) 0.051 Uiso 1 1 d D
C7 C -0.0126(5) 0.5855(6) 0.1773(4) 0.0400(15) Uani 1 1 d D
H7A H -0.101(2) 0.606(5) 0.124(4) 0.048 Uiso 1 1 d D
H7B H 0.035(4) 0.658(4) 0.157(4) 0.048 Uiso 1 1 d 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 0.0000 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'
Mg Mg 0.0486 0.0363 '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
O1 Mg1 C2 107.36(15) . 2
O1 Mg1 C2 107.36(15) . .
C2 Mg1 C2 145.3(3) 2 .
O1 Mg1 C1 83.01(14) . .
C2 Mg1 C1 155.70(17) 2 .
C2 Mg1 C1 32.99(18) . .
O1 Mg1 C1 83.01(14) . 2
C2 Mg1 C1 32.99(18) 2 2
C2 Mg1 C1 155.70(17) . 2
C1 Mg1 C1 166.0(3) . 2
O1 Mg1 C4 126.58(16) . .
C2 Mg1 C4 102.5(2) 2 .
C2 Mg1 C4 55.08(18) . .
C1 Mg1 C4 55.4(2) . .
C1 Mg1 C4 135.5(2) 2 .
O1 Mg1 C4 126.58(16) . 2
C2 Mg1 C4 55.08(18) 2 2
C2 Mg1 C4 102.5(2) . 2
C1 Mg1 C4 135.5(2) . 2
C1 Mg1 C4 55.4(2) 2 2
C4 Mg1 C4 106.8(3) . 2
O1 Mg1 C5 93.46(15) . 2
C2 Mg1 C5 55.34(19) 2 2
C2 Mg1 C5 122.2(2) . 2
C1 Mg1 C5 147.79(17) . 2
C1 Mg1 C5 33.76(18) 2 2
C4 Mg1 C5 139.8(3) . 2
C4 Mg1 C5 33.36(18) 2 2
O1 Mg1 C5 93.46(15) . .
C2 Mg1 C5 122.2(2) 2 .
C2 Mg1 C5 55.34(19) . .
C1 Mg1 C5 33.76(18) . .
C1 Mg1 C5 147.79(17) 2 .
C4 Mg1 C5 33.36(18) . .
C4 Mg1 C5 139.8(3) 2 .
C5 Mg1 C5 173.1(3) 2 .
O1 Mg1 C3 137.99(15) . 2
C2 Mg1 C3 33.28(17) 2 2
C2 Mg1 C3 113.1(2) . 2
C1 Mg1 C3 138.6(2) . 2
C1 Mg1 C3 55.3(2) 2 2
C4 Mg1 C3 87.1(2) . 2
C4 Mg1 C3 33.35(16) 2 2
C5 Mg1 C3 55.53(19) 2 2
C5 Mg1 C3 118.4(2) . 2
O1 Mg1 C3 137.99(15) . .
C2 Mg1 C3 113.1(2) 2 .
C2 Mg1 C3 33.28(17) . .
C1 Mg1 C3 55.3(2) . .
C1 Mg1 C3 138.6(2) 2 .
C4 Mg1 C3 33.35(16) . .
C4 Mg1 C3 87.1(2) 2 .
C5 Mg1 C3 118.4(2) 2 .
C5 Mg1 C3 55.53(19) . .
C3 Mg1 C3 84.0(3) 2 .
C2 C1 C5 107.9(5) . .
C2 C1 Mg1 73.1(3) . .
C5 C1 Mg1 73.6(3) . .
C2 C1 H1 133(3) . .
C5 C1 H1 119(3) . .
Mg1 C1 H1 116(3) . .
C1 C2 C3 109.7(4) . .
C1 C2 Mg1 73.9(3) . .
C3 C2 Mg1 74.9(3) . .
C1 C2 H2 113(3) . .
C3 C2 H2 137(3) . .
Mg1 C2 H2 120(3) . .
C2 C3 C4 106.5(5) . .
C2 C3 Mg1 71.8(3) . .
C4 C3 Mg1 72.5(3) . .
C2 C3 H3 128(3) . .
C4 C3 H3 125(3) . .
Mg1 C3 H3 121(3) . .
C5 C4 C3 108.9(4) . .
C5 C4 Mg1 73.5(3) . .
C3 C4 Mg1 74.2(3) . .
C5 C4 H4 127(3) . .
C3 C4 H4 124(3) . .
Mg1 C4 H4 119(3) . .
C4 C5 C1 106.9(4) . .
C4 C5 Mg1 73.2(3) . .
C1 C5 Mg1 72.6(3) . .
C4 C5 H5 133(3) . .
C1 C5 H5 120(3) . .
Mg1 C5 H5 124(3) . .
C6 O1 C6 107.2(5) 2 .
C6 O1 Mg1 126.4(3) 2 .
C6 O1 Mg1 126.4(3) . .
O1 C6 C7 106.7(4) . .
O1 C6 H6A 101(3) . .
C7 C6 H6A 115(3) . .
O1 C6 H6B 114(3) . .
C7 C6 H6B 109(3) . .
H6A C6 H6B 110(4) . .
C6 C7 C7 101.6(3) . 2
C6 C7 H7A 116(3) . .
C7 C7 H7A 107(3) 2 .
C6 C7 H7B 112(3) . .
C7 C7 H7B 113(3) 2 .
H7A C7 H7B 107(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O1 2.093(6) .
Mg1 C2 2.441(6) 2
Mg1 C2 2.441(6) .
Mg1 C1 2.451(7) .
Mg1 C1 2.451(7) 2
Mg1 C4 2.460(6) .
Mg1 C4 2.460(6) 2
Mg1 C5 2.464(6) 2
Mg1 C5 2.464(6) .
Mg1 C3 2.482(6) 2
Mg1 C3 2.482(6) .
C1 C2 1.389(7) .
C1 C5 1.427(7) .
C1 H1 0.96(2) .
C2 C3 1.410(7) .
C2 H2 0.96(2) .
C3 C4 1.418(7) .
C3 H3 0.96(2) .
C4 C5 1.413(8) .
C4 H4 0.96(2) .
C5 H5 0.96(2) .
O1 C6 1.484(6) 2
O1 C6 1.484(6) .
C6 C7 1.505(8) .
C6 H6A 1.01(2) .
C6 H6B 1.01(2) .
C7 C7 1.565(8) 2
C7 H7A 1.01(2) .
C7 H7B 1.01(2) .
