#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:29:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179181 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/29/4312961.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_4312961
loop_
_publ_author_name
'Renata Dreos'
'Giorgio Nardin'
'Lucio Randaccio'
'Patrizia Siega'
'Giovanni Tauzher'
_publ_section_title
;
 A Guest-Induced Assembly of a Molecular Box from Methylcobaloxime and
 1,4-Phenylenebisboronic Acid
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              612
_journal_page_last               617
_journal_paper_doi               10.1021/ic025909s
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '(C15 H25 B2 Co N4 O8),3(H2 O)'
_chemical_formula_sum            'C15 H31 B2 Co N4 O11'
_chemical_formula_weight         523.99
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.24(2)
_cell_angle_beta                 111.199(15)
_cell_angle_gamma                97.834(18)
_cell_formula_units_Z            2
_cell_length_a                   8.853(3)
_cell_length_b                   11.865(4)
_cell_length_c                   12.866(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1166.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7638
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.140
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0748P)²+0.5594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                4125
_reflns_number_total             4677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025909s_3.cif
_cod_data_source_block           codib2-compound3
_cod_database_code               4312961
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1476(3) -0.0340(2) 0.1773(2) 0.0339(5) Uani 1 1 d . . .
H1A H 0.0392 -0.0896 0.1246 0.051 Uiso 1 1 calc R . .
H1B H 0.1987 -0.0590 0.2438 0.051 Uiso 1 1 calc R . .
H1C H 0.2175 -0.0339 0.1351 0.051 Uiso 1 1 calc R . .
C2 C 0.1277(3) 0.0910(2) 0.2216(2) 0.0285(5) Uani 1 1 d . . .
C15 C -0.1291(3) 0.2597(3) 0.1260(2) 0.0352(5) Uani 1 1 d . . .
H15A H -0.1914 0.3155 0.1468 0.053 Uiso 1 1 calc R . .
H15B H -0.1752 0.1819 0.1267 0.053 Uiso 1 1 calc R . .
H15C H -0.1363 0.2508 0.0478 0.053 Uiso 1 1 calc R . .
C3 C 0.0761(3) 0.1332(2) 0.3200(2) 0.0289(5) Uani 1 1 d . . .
C4 C 0.0457(3) 0.0571(3) 0.3891(2) 0.0387(6) Uani 1 1 d . . .
H4A H 0.0101 0.1016 0.4468 0.058 Uiso 1 1 calc R . .
H4B H 0.1475 0.0376 0.4295 0.058 Uiso 1 1 calc R . .
H4C H -0.0403 -0.0167 0.3356 0.058 Uiso 1 1 calc R . .
C5 C 0.1933(3) 0.5952(2) 0.1077(2) 0.0350(5) Uani 1 1 d . . .
H5A H 0.2203 0.5499 0.0454 0.052 Uiso 1 1 calc R . .
H5B H 0.2876 0.6631 0.1637 0.052 Uiso 1 1 calc R . .
H5C H 0.0978 0.6243 0.0739 0.052 Uiso 1 1 calc R . .
C6 C 0.1533(3) 0.5149(2) 0.1703(2) 0.0278(5) Uani 1 1 d . . .
C7 C 0.0991(3) 0.5575(2) 0.2673(2) 0.0300(5) Uani 1 1 d . . .
C8 C 0.0797(3) 0.6827(2) 0.3112(2) 0.0359(5) Uani 1 1 d . . .
H8A H 0.0563 0.6933 0.3801 0.054 Uiso 1 1 calc R . .
H8B H -0.0113 0.6939 0.2496 0.054 Uiso 1 1 calc R . .
H8C H 0.1818 0.7415 0.3323 0.054 Uiso 1 1 calc R . .
C9 C 0.3315(3) 0.2031(2) -0.0410(2) 0.0302(5) Uani 1 1 d . . .
C10 C 0.3653(3) 0.0902(2) -0.0720(2) 0.0359(5) Uani 1 1 d . . .
H10 H 0.3625 0.0426 -0.0259 0.043 Uiso 1 1 calc R . .
C11 C 0.4029(3) 0.0459(3) -0.1691(2) 0.0367(5) Uani 1 1 d . . .
H11 H 0.4254 -0.0298 -0.1861 0.044 Uiso 1 1 calc R . .
C12 C 0.4074(3) 0.1140(2) -0.2421(2) 0.0307(5) Uani 1 1 d . . .
C13 C 0.3726(3) 0.2258(2) -0.2124(2) 0.0356(5) Uani 1 1 d . . .
H13 H 0.3735 0.2728 -0.2593 0.043 Uiso 1 1 calc R . .
C14 C 0.3360(3) 0.2705(2) -0.1140(2) 0.0356(5) Uani 1 1 d . . .
H14 H 0.3142 0.3464 -0.0967 0.043 Uiso 1 1 calc R . .
B1 B 0.2969(3) 0.2542(3) 0.0759(2) 0.0299(5) Uani 1 1 d . . .
B2 B 0.4493(3) 0.0657(3) -0.3535(2) 0.0322(6) Uani 1 1 d . . .
N1 N 0.1509(2) 0.17446(18) 0.17810(16) 0.0279(4) Uani 1 1 d . . .
N2 N 0.1613(2) 0.40309(19) 0.14822(17) 0.0275(4) Uani 1 1 d . . .
N3 N 0.0729(3) 0.47330(19) 0.30987(17) 0.0299(4) Uani 1 1 d . . .
N4 N 0.0615(2) 0.24349(19) 0.33960(17) 0.0301(4) Uani 1 1 d . . .
O1 O 0.1927(2) 0.14557(15) 0.08259(14) 0.0297(4) Uani 1 1 d . . .
O2 O 0.2018(2) 0.34865(16) 0.05621(14) 0.0298(4) Uani 1 1 d . . .
O2W O 0.4611(2) 0.36986(17) 0.58100(16) 0.0402(4) Uani 1 1 d . . .
O1W O 0.3610(2) 0.39441(16) 0.36514(14) 0.0322(4) Uani 1 1 d . . .
O3 O 0.0232(2) 0.49671(17) 0.39994(16) 0.0368(4) Uani 1 1 d . . .
H3 H 0.0109 0.4359 0.4177 0.055 Uiso 1 1 calc . . .
O3W O 0.3363(2) -0.24003(19) -0.36510(19) 0.0453(5) Uani 1 1 d . . .
O4 O 0.0157(2) 0.29820(17) 0.42705(15) 0.0351(4) Uani 1 1 d . . .
O4W O 0.6953(2) 0.51558(19) 0.27875(19) 0.0469(5) Uani 1 1 d . . .
O5 O 0.4482(2) 0.30640(16) 0.18930(14) 0.0319(4) Uani 1 1 d . . .
O6 O 0.4974(2) 0.14902(17) -0.39904(16) 0.0377(4) Uani 1 1 d . . .
H6 H 0.5166 0.1143 -0.4558 0.057 Uiso 1 1 calc . . .
O7 O 0.4417(2) -0.04919(17) -0.40661(15) 0.0368(4) Uani 1 1 d . . .
H7 H 0.4112 -0.0912 -0.3732 0.055 Uiso 1 1 calc . . .
Co Co 0.11125(4) 0.32380(3) 0.24415(2) 0.02597(13) Uani 1 1 d . . .
H1O5 H 0.5195 0.3759 0.1910 0.050 Uiso 1 1 d . . .
H2W1 H 0.4074 0.3614 0.3168 0.050 Uiso 1 1 d . . .
H1W1 H 0.3882 0.3763 0.4201 0.050 Uiso 1 1 d . . .
H1W2 H 0.4967 0.3034 0.5923 0.050 Uiso 1 1 d . . .
H1W3 H 0.2270 -0.2749 -0.3925 0.050 Uiso 1 1 d . . .
H2W3 H 0.3958 -0.2614 -0.3020 0.050 Uiso 1 1 d . . .
H1W4 H 0.7904 0.5080 0.3250 0.050 Uiso 1 1 d . . .
H2W4 H 0.6628 0.5555 0.3357 0.050 Uiso 1 1 d . . .
H2W2 H 0.5426 0.4368 0.5843 0.050 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
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Co Co 0.3494 0.9721 '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
_geom_angle_publ_flag
N1 C2 C3 112.0(2) . . ?
N1 C2 C1 124.5(2) . . ?
C3 C2 C1 123.4(2) . . ?
N4 C3 C2 112.2(2) . . ?
N4 C3 C4 124.1(2) . . ?
C2 C3 C4 123.7(2) . . ?
N2 C6 C7 112.4(2) . . ?
N2 C6 C5 125.6(2) . . ?
C7 C6 C5 122.1(2) . . ?
N3 C7 C6 111.7(2) . . ?
N3 C7 C8 124.5(2) . . ?
C6 C7 C8 123.7(2) . . ?
C10 C9 C14 116.3(2) . . ?
C10 C9 B1 121.1(2) . . ?
C14 C9 B1 122.5(2) . . ?
C11 C10 C9 122.5(2) . . ?
C10 C11 C12 120.9(3) . . ?
C13 C12 C11 116.9(2) . . ?
C13 C12 B2 121.1(2) . . ?
C11 C12 B2 122.0(2) . . ?
C12 C13 C14 122.0(2) . . ?
C13 C14 C9 121.3(3) . . ?
O5 B1 O2 110.6(2) . . ?
O5 B1 O1 106.63(19) . . ?
O2 B1 O1 112.32(19) . . ?
O5 B1 C9 114.95(19) . . ?
O2 B1 C9 106.03(19) . . ?
O1 B1 C9 106.4(2) . . ?
O7 B2 O6 117.2(2) . . ?
O7 B2 C12 125.0(2) . . ?
O6 B2 C12 117.8(2) . . ?
C2 N1 O1 118.0(2) . . ?
C2 N1 Co 117.28(16) . . ?
O1 N1 Co 124.58(15) . . ?
C6 N2 O2 119.12(19) . . ?
C6 N2 Co 116.93(16) . . ?
O2 N2 Co 123.94(16) . . ?
C7 N3 O3 119.8(2) . . ?
C7 N3 Co 117.32(16) . . ?
O3 N3 Co 122.87(15) . . ?
C3 N4 O4 120.8(2) . . ?
C3 N4 Co 116.91(16) . . ?
O4 N4 Co 122.26(16) . . ?
N1 O1 B1 113.63(17) . . ?
N2 O2 B1 114.32(17) . . ?
N3 Co N1 179.63(8) . . ?
N3 Co N2 81.61(9) . . ?
N1 Co N2 98.08(9) . . ?
N3 Co N4 98.77(9) . . ?
N1 Co N4 81.53(9) . . ?
N2 Co N4 179.61(8) . . ?
N3 Co C15 90.53(11) . . ?
N1 Co C15 89.68(10) . . ?
N2 Co C15 90.50(10) . . ?
N4 Co C15 89.49(10) . . ?
N3 Co O1W 88.52(8) . . ?
N1 Co O1W 91.26(8) . . ?
N2 Co O1W 88.10(8) . . ?
N4 Co O1W 91.91(8) . . ?
C15 Co O1W 178.41(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.493(3) . ?
C2 N1 1.293(3) . ?
C2 C3 1.480(3) . ?
C15 Co 1.998(3) . ?
C3 N4 1.296(3) . ?
C3 C4 1.495(3) . ?
C5 C6 1.491(3) . ?
C6 N2 1.294(3) . ?
C6 C7 1.480(3) . ?
C7 N3 1.299(3) . ?
C7 C8 1.492(3) . ?
C9 C10 1.392(4) . ?
C9 C14 1.401(3) . ?
C9 B1 1.612(3) . ?
C10 C11 1.390(3) . ?
C11 C12 1.406(3) . ?
C12 C13 1.384(4) . ?
C12 B2 1.583(3) . ?
C13 C14 1.398(3) . ?
B1 O5 1.470(3) . ?
B1 O2 1.513(3) . ?
B1 O1 1.521(3) . ?
B2 O7 1.323(4) . ?
B2 O6 1.375(3) . ?
N1 O1 1.376(2) . ?
N1 Co 1.878(2) . ?
N2 O2 1.375(2) . ?
N2 Co 1.880(2) . ?
N3 O3 1.355(2) . ?
N3 Co 1.874(2) . ?
N4 O4 1.358(2) . ?
N4 Co 1.882(2) . ?
O1W Co 2.0712(18) . ?
