#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:51:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178758 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/12/4101273.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_4101273
loop_
_publ_author_name
'Kawano, Masaki'
'Kobayashi, Yasuhiro'
'Ozeki, Tomoji'
'Fujita, Makoto'
_publ_contact_author             'Masaki Kawano'
_publ_section_title
;
 Direct crystallographic observation of a coordinatively unsaturated
 transition-metal complex in situ generated within a self-assembled
 cage.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6558
_journal_page_last               6559
_journal_paper_doi               10.1021/ja0609250
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C8 H5 Mn O3'
_chemical_formula_weight         204.06
_chemical_name_systematic
; 
 ? 
;
_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                 115.7200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7492(3)
_cell_length_b                   6.9262(2)
_cell_length_c                   11.6456(3)
_cell_measurement_reflns_used    6430
_cell_measurement_temperature    78(2)
_cell_measurement_theta_max      37.6
_cell_measurement_theta_min      3.4
_cell_volume                     781.13(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker XSHELL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      78(2)
_diffrn_measured_fraction_theta_full 0.765
_diffrn_measured_fraction_theta_max 0.765
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       omega_scan
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12521
_diffrn_reflns_theta_full        37.61
_diffrn_reflns_theta_max         37.61
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_T_max  0.8270
_exptl_absorpt_correction_T_min  0.5967
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         3170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0249
_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)+(0.0364P)²+0.1173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                2532
_reflns_number_total             3170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0609250si20060208_045957.cif
_cod_data_source_block           CpMn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4101273
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
Mn1 Mn 0.472075(16) 1.003725(19) 0.708505(14) 0.01028(5) Uani 1 1 d
C1 C 0.33114(12) 0.87889(15) 0.77332(11) 0.0168(2) Uani 1 1 d
H1 H 0.3036(17) 0.940(3) 0.8297(15) 0.029(4) Uiso 1 1 d
C2 C 0.26373(11) 0.90178(15) 0.63978(11) 0.0155(2) Uani 1 1 d
H2 H 0.1882(18) 0.979(2) 0.5913(16) 0.024(4) Uiso 1 1 d
C3 C 0.33576(12) 0.78805(15) 0.58537(11) 0.0169(2) Uani 1 1 d
H3 H 0.3145(16) 0.779(2) 0.5009(14) 0.023(4) Uiso 1 1 d
C4 C 0.44701(12) 0.69660(15) 0.68623(11) 0.0178(2) Uani 1 1 d
H4 H 0.5113(16) 0.616(2) 0.6768(14) 0.026(4) Uiso 1 1 d
C5 C 0.44533(12) 0.75273(15) 0.80284(11) 0.0176(2) Uani 1 1 d
H5 H 0.5095(16) 0.714(2) 0.8835(14) 0.026(4) Uiso 1 1 d
O6 O 0.56107(9) 1.28899(13) 0.91641(8) 0.02250(18) Uani 1 1 d
C6 C 0.52725(11) 1.17829(14) 0.83479(10) 0.01486(19) Uani 1 1 d
O7 O 0.39657(10) 1.30942(12) 0.51290(8) 0.02232(17) Uani 1 1 d
C7 C 0.42686(12) 1.19038(14) 0.58893(10) 0.01500(19) Uani 1 1 d
O8 O 0.75486(10) 0.96285(13) 0.73081(10) 0.0260(2) Uani 1 1 d
C8 C 0.64465(13) 0.98094(14) 0.72166(11) 0.0169(2) 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 0.0033 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'
Mn Mn 0.3368 0.7283 '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
C6 Mn1 C8 91.57(5)
C6 Mn1 C7 91.85(5)
C8 Mn1 C7 92.92(5)
C6 Mn1 C5 101.35(4)
C8 Mn1 C5 104.35(5)
C7 Mn1 C5 157.80(5)
C6 Mn1 C2 116.61(4)
C8 Mn1 C2 150.84(4)
C7 Mn1 C2 93.44(5)
C5 Mn1 C2 64.74(4)
C6 Mn1 C4 138.30(5)
C8 Mn1 C4 89.66(4)
C7 Mn1 C4 129.72(4)
C5 Mn1 C4 38.69(4)
C2 Mn1 C4 64.69(4)
C6 Mn1 C1 90.91(4)
C8 Mn1 C1 142.48(5)
C7 Mn1 C1 124.40(5)
C5 Mn1 C1 38.74(4)
C2 Mn1 C1 38.40(4)
C4 Mn1 C1 64.68(4)
C6 Mn1 C3 154.58(4)
C8 Mn1 C3 112.03(4)
C7 Mn1 C3 96.07(5)
C5 Mn1 C3 64.74(4)
C2 Mn1 C3 38.95(4)
C4 Mn1 C3 38.39(5)
C1 Mn1 C3 64.74(4)
C2 C1 C5 108.19(9)
C2 C1 Mn1 70.75(6)
C5 C1 Mn1 70.46(6)
C1 C2 C3 107.97(10)
C1 C2 Mn1 70.85(6)
C3 C2 Mn1 70.63(6)
C4 C3 C2 107.72(10)
C4 C3 Mn1 70.75(6)
C2 C3 Mn1 70.42(6)
C3 C4 C5 108.37(9)
C3 C4 Mn1 70.87(6)
C5 C4 Mn1 70.49(6)
C4 C5 C1 107.75(10)
C4 C5 Mn1 70.82(6)
C1 C5 Mn1 70.80(6)
O6 C6 Mn1 178.86(9)
O7 C7 Mn1 179.17(10)
O8 C8 Mn1 178.70(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 C6 1.7942(10)
Mn1 C8 1.8008(12)
Mn1 C7 1.8053(11)
Mn1 C5 2.1415(10)
Mn1 C2 2.1445(11)
Mn1 C4 2.1458(10)
Mn1 C1 2.1459(10)
Mn1 C3 2.1473(11)
C1 C2 1.4109(16)
C1 C5 1.4220(16)
C2 C3 1.4309(15)
C3 C4 1.4113(17)
C4 C5 1.4202(16)
O6 C6 1.1505(13)
O7 C7 1.1487(13)
O8 C8 1.1494(15)
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
C6 Mn1 C1 C2 134.52(7)
C8 Mn1 C1 C2 -131.70(8)
C7 Mn1 C1 C2 41.66(8)
C5 Mn1 C1 C2 -118.34(9)
C4 Mn1 C1 C2 -80.54(7)
C3 Mn1 C1 C2 -37.89(6)
C6 Mn1 C1 C5 -107.13(7)
C8 Mn1 C1 C5 -13.36(11)
C7 Mn1 C1 C5 160.00(7)
C2 Mn1 C1 C5 118.34(9)
C4 Mn1 C1 C5 37.81(7)
C3 Mn1 C1 C5 80.45(7)
C5 C1 C2 C3 0.39(12)
Mn1 C1 C2 C3 61.21(7)
C5 C1 C2 Mn1 -60.82(7)
C6 Mn1 C2 C1 -52.88(7)
C8 Mn1 C2 C1 111.07(10)
C7 Mn1 C2 C1 -146.67(6)
C5 Mn1 C2 C1 37.52(6)
C4 Mn1 C2 C1 80.50(7)
C3 Mn1 C2 C1 117.92(9)
C6 Mn1 C2 C3 -170.79(6)
C8 Mn1 C2 C3 -6.85(13)
C7 Mn1 C2 C3 95.41(7)
C5 Mn1 C2 C3 -80.40(7)
C4 Mn1 C2 C3 -37.41(6)
C1 Mn1 C2 C3 -117.92(9)
C1 C2 C3 C4 -0.11(12)
Mn1 C2 C3 C4 61.24(7)
C1 C2 C3 Mn1 -61.35(7)
C6 Mn1 C3 C4 -98.34(11)
C8 Mn1 C3 C4 58.60(7)
C7 Mn1 C3 C4 154.24(7)
C5 Mn1 C3 C4 -37.42(6)
C2 Mn1 C3 C4 -117.81(9)
C1 Mn1 C3 C4 -80.44(7)
C6 Mn1 C3 C2 19.47(14)
C8 Mn1 C3 C2 176.41(7)
C7 Mn1 C3 C2 -87.95(7)
C5 Mn1 C3 C2 80.39(7)
C4 Mn1 C3 C2 117.81(9)
C1 Mn1 C3 C2 37.36(6)
C2 C3 C4 C5 -0.22(12)
Mn1 C3 C4 C5 60.81(7)
C2 C3 C4 Mn1 -61.03(7)
C6 Mn1 C4 C3 140.32(7)
C8 Mn1 C4 C3 -127.70(7)
C7 Mn1 C4 C3 -34.18(9)
C5 Mn1 C4 C3 118.48(9)
C2 Mn1 C4 C3 37.96(6)
C1 Mn1 C4 C3 80.62(7)
C6 Mn1 C4 C5 21.85(10)
C8 Mn1 C4 C5 113.83(7)
C7 Mn1 C4 C5 -152.66(7)
C2 Mn1 C4 C5 -80.52(7)
C1 Mn1 C4 C5 -37.85(7)
C3 Mn1 C4 C5 -118.48(9)
C3 C4 C5 C1 0.46(12)
Mn1 C4 C5 C1 61.51(7)
C3 C4 C5 Mn1 -61.05(7)
C2 C1 C5 C4 -0.52(12)
Mn1 C1 C5 C4 -61.52(7)
C2 C1 C5 Mn1 61.00(7)
C6 Mn1 C5 C4 -165.38(7)
C8 Mn1 C5 C4 -70.77(8)
C7 Mn1 C5 C4 69.26(13)
C2 Mn1 C5 C4 80.39(7)
C1 Mn1 C5 C4 117.58(10)
C3 Mn1 C5 C4 37.12(7)
C6 Mn1 C5 C1 77.04(7)
C8 Mn1 C5 C1 171.65(7)
C7 Mn1 C5 C1 -48.32(14)
C2 Mn1 C5 C1 -37.19(7)
C4 Mn1 C5 C1 -117.58(10)
C3 Mn1 C5 C1 -80.46(7)
C8 Mn1 C6 O6 -145(6)
C7 Mn1 C6 O6 122(6)
C5 Mn1 C6 O6 -40(6)
C2 Mn1 C6 O6 27(6)
C4 Mn1 C6 O6 -54(6)
C1 Mn1 C6 O6 -2(6)
C3 Mn1 C6 O6 14(6)
C6 Mn1 C7 O7 -83(7)
C8 Mn1 C7 O7 -175(100)
C5 Mn1 C7 O7 44(7)
C2 Mn1 C7 O7 34(7)
C4 Mn1 C7 O7 93(7)
C1 Mn1 C7 O7 9(7)
C3 Mn1 C7 O7 73(7)
C6 Mn1 C8 O8 114(5)
C7 Mn1 C8 O8 -154(5)
C5 Mn1 C8 O8 12(5)
C2 Mn1 C8 O8 -51(5)
C4 Mn1 C8 O8 -24(5)
C1 Mn1 C8 O8 21(5)
C3 Mn1 C8 O8 -56(5)
