#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:37:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178908 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/37/4113761.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_4113761
loop_
_publ_author_name
'Catherine Bergquist'
'Tauqir Fillebeen'
'Melissa M. Morlok'
'Gerard Parkin'
_publ_section_title
;
 Protonation and Reactivity towards Carbon Dioxide of the Mononuclear
 Tetrahedral Zinc and Cobalt Hydroxide Complexes, [TpBut,Me]ZnOH and
 [TpBut,Me]CoOH: Comparison of the Reactivity of the Metal Hydroxide
 Function in Synthetic Analogues of Carbonic Anhydrase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6189
_journal_page_last               6199
_journal_paper_doi               10.1021/ja034711j
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C24 H38 B Co N6 O'
_chemical_formula_weight         496.34
_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                 100.9100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5712(8)
_cell_length_b                   30.523(2)
_cell_length_c                   9.5763(7)
_cell_measurement_temperature    238(2)
_cell_volume                     2747.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      238(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.1159
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19295
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.9378
_exptl_absorpt_correction_T_min  0.8809
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0635P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                3191
_reflns_number_total             6341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034711jsi20030217_102458.cif
_cod_data_source_block           ts10
_cod_database_code               4113761
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
Co Co 0.48171(5) 0.141052(17) 0.48376(5) 0.03799(18) Uani 1 1 d .
O O 0.5075(3) 0.15595(11) 0.3022(3) 0.0723(10) Uani 1 1 d .
H0A H 0.5552 0.1788 0.3060 0.108 Uiso 1 1 calc R
N1 N 0.3669(3) 0.08097(9) 0.6612(3) 0.0342(7) Uani 1 1 d .
N2 N 0.3687(3) 0.08632(10) 0.5183(3) 0.0380(7) Uani 1 1 d .
N3 N 0.3850(3) 0.16004(9) 0.7401(3) 0.0332(7) Uani 1 1 d .
N4 N 0.3836(3) 0.17937(9) 0.6097(3) 0.0356(7) Uani 1 1 d .
N5 N 0.6058(3) 0.11357(9) 0.7660(3) 0.0353(7) Uani 1 1 d .
N6 N 0.6501(3) 0.12637(9) 0.6427(3) 0.0375(7) Uani 1 1 d .
C11 C 0.2666(5) 0.03049(14) 0.8212(4) 0.0629(13) Uani 1 1 d .
H11A H 0.3576 0.0245 0.8823 0.094 Uiso 1 1 calc R
H11B H 0.2088 0.0042 0.8110 0.094 Uiso 1 1 calc R
H11C H 0.2181 0.0535 0.8632 0.094 Uiso 1 1 calc R
C12 C 0.2901(4) 0.04486(12) 0.6788(4) 0.0434(10) Uani 1 1 d .
C13 C 0.2414(4) 0.02645(13) 0.5472(4) 0.0502(11) Uani 1 1 d .
C14 C 0.2924(4) 0.05353(12) 0.4500(4) 0.0431(10) Uani 1 1 d .
C15 C 0.2714(5) 0.04855(14) 0.2892(4) 0.0559(12) Uani 1 1 d .
C16 C 0.1754(8) 0.00933(18) 0.2424(6) 0.134(3) Uani 1 1 d .
H16A H 0.2271 -0.0175 0.2711 0.201 Uiso 1 1 calc R
H16B H 0.1456 0.0097 0.1398 0.201 Uiso 1 1 calc R
H16C H 0.0923 0.0108 0.2865 0.201 Uiso 1 1 calc R
C17 C 0.4172(6) 0.0419(2) 0.2474(5) 0.115(2) Uani 1 1 d .
H17A H 0.4771 0.0672 0.2775 0.173 Uiso 1 1 calc R
H17B H 0.4048 0.0387 0.1450 0.173 Uiso 1 1 calc R
H17C H 0.4618 0.0158 0.2933 0.173 Uiso 1 1 calc R
C18 C 0.1993(5) 0.08817(16) 0.2171(4) 0.0728(14) Uani 1 1 d .
H18A H 0.1138 0.0943 0.2543 0.109 Uiso 1 1 calc R
H18B H 0.1740 0.0829 0.1155 0.109 Uiso 1 1 calc R
H18C H 0.2631 0.1131 0.2346 0.109 Uiso 1 1 calc R
C21 C 0.3050(5) 0.17626(14) 0.9682(4) 0.0536(11) Uani 1 1 d .
H21A H 0.2363 0.1527 0.9646 0.080 Uiso 1 1 calc R
H21B H 0.2711 0.2019 1.0118 0.080 Uiso 1 1 calc R
H21C H 0.3955 0.1670 1.0241 0.080 Uiso 1 1 calc R
C22 C 0.3233(4) 0.18720(12) 0.8221(4) 0.0386(9) Uani 1 1 d .
C23 C 0.2793(4) 0.22452(12) 0.7438(4) 0.0446(10) Uani 1 1 d .
C24 C 0.3195(4) 0.21837(11) 0.6123(4) 0.0368(9) Uani 1 1 d .
C25 C 0.2983(4) 0.24964(13) 0.4854(5) 0.0535(11) Uani 1 1 d .
C26 C 0.2071(6) 0.28812(16) 0.5166(6) 0.0976(19) Uani 1 1 d .
H26A H 0.1175 0.2773 0.5359 0.146 Uiso 1 1 calc R
H26B H 0.1890 0.3075 0.4349 0.146 Uiso 1 1 calc R
H26C H 0.2569 0.3041 0.5987 0.146 Uiso 1 1 calc R
C27 C 0.2222(5) 0.22618(16) 0.3525(4) 0.0704(14) Uani 1 1 d .
H27A H 0.2785 0.2012 0.3334 0.106 Uiso 1 1 calc R
H27B H 0.2099 0.2462 0.2724 0.106 Uiso 1 1 calc R
H27C H 0.1298 0.2162 0.3670 0.106 Uiso 1 1 calc R
C28 C 0.4445(5) 0.26603(16) 0.4644(5) 0.0794(16) Uani 1 1 d .
H28A H 0.4921 0.2807 0.5501 0.119 Uiso 1 1 calc R
H28B H 0.4323 0.2864 0.3852 0.119 Uiso 1 1 calc R
H28C H 0.5015 0.2414 0.4444 0.119 Uiso 1 1 calc R
C31 C 0.7093(4) 0.08845(14) 1.0107(4) 0.0569(12) Uani 1 1 d .
H31A H 0.8036 0.0843 1.0676 0.085 Uiso 1 1 calc R
H31B H 0.6580 0.0609 1.0034 0.085 Uiso 1 1 calc R
H31C H 0.6582 0.1101 1.0555 0.085 Uiso 1 1 calc R
C32 C 0.7217(4) 0.10371(11) 0.8663(4) 0.0391(9) Uani 1 1 d .
C33 C 0.8413(4) 0.11023(12) 0.8088(4) 0.0435(10) Uani 1 1 d .
C34 C 0.7926(4) 0.12439(11) 0.6691(4) 0.0368(9) Uani 1 1 d .
C35 C 0.8775(4) 0.13690(13) 0.5554(4) 0.0460(10) Uani 1 1 d .
C36 C 0.8490(5) 0.18450(14) 0.5131(5) 0.0658(13) Uani 1 1 d .
H36A H 0.7487 0.1883 0.4734 0.099 Uiso 1 1 calc R
H36B H 0.9050 0.1926 0.4426 0.099 Uiso 1 1 calc R
H36C H 0.8750 0.2030 0.5962 0.099 Uiso 1 1 calc R
C37 C 0.8367(5) 0.10730(16) 0.4263(5) 0.0718(14) Uani 1 1 d .
H37A H 0.8594 0.0772 0.4538 0.108 Uiso 1 1 calc R
H37B H 0.8892 0.1160 0.3536 0.108 Uiso 1 1 calc R
H37C H 0.7355 0.1099 0.3894 0.108 Uiso 1 1 calc R
C38 C 1.0362(4) 0.13136(16) 0.6168(5) 0.0734(15) Uani 1 1 d .
H38A H 1.0622 0.1498 0.7002 0.110 Uiso 1 1 calc R
H38B H 1.0913 0.1398 0.5460 0.110 Uiso 1 1 calc R
H38C H 1.0557 0.1010 0.6432 0.110 Uiso 1 1 calc R
B B 0.4456(4) 0.11360(13) 0.7716(4) 0.0340(10) Uani 1 1 d .
H1 H 0.433(3) 0.1037(8) 0.872(3) 0.012(7) 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'
H H 0.0000 0.0000 '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
O Co N4 124.91(13)
O Co N6 121.61(12)
N4 Co N6 94.13(12)
O Co N2 121.18(13)
N4 Co N2 93.22(11)
N6 Co N2 93.84(12)
C12 N1 N2 109.1(3)
C12 N1 B 130.4(3)
N2 N1 B 120.5(3)
C14 N2 N1 106.8(3)
C14 N2 Co 142.0(3)
N1 N2 Co 111.2(2)
C22 N3 N4 109.5(3)
C22 N3 B 129.8(3)
N4 N3 B 120.6(3)
C24 N4 N3 106.8(3)
C24 N4 Co 141.8(2)
N3 N4 Co 111.4(2)
C32 N5 N6 109.0(3)
C32 N5 B 131.3(3)
N6 N5 B 119.7(3)
C34 N6 N5 106.9(3)
C34 N6 Co 141.3(3)
N5 N6 Co 111.8(2)
N1 C12 C13 108.4(3)
N1 C12 C11 122.2(4)
C13 C12 C11 129.3(4)
C12 C13 C14 105.5(4)
N2 C14 C13 110.1(3)
N2 C14 C15 121.7(4)
C13 C14 C15 128.1(4)
C18 C15 C14 110.3(3)
C18 C15 C16 107.4(4)
C14 C15 C16 109.5(4)
C18 C15 C17 110.4(4)
C14 C15 C17 108.9(4)
C16 C15 C17 110.3(5)
N3 C22 C23 108.1(3)
N3 C22 C21 123.6(3)
C23 C22 C21 128.2(3)
C22 C23 C24 105.7(3)
N4 C24 C23 109.9(3)
N4 C24 C25 122.1(3)
C23 C24 C25 127.9(3)
C27 C25 C26 109.0(4)
C27 C25 C24 110.0(3)
C26 C25 C24 108.7(4)
C27 C25 C28 110.3(4)
C26 C25 C28 110.1(4)
C24 C25 C28 108.7(3)
N5 C32 C33 108.4(3)
N5 C32 C31 122.0(3)
C33 C32 C31 129.6(4)
C32 C33 C34 106.0(3)
N6 C34 C33 109.7(3)
N6 C34 C35 121.0(3)
C33 C34 C35 129.3(3)
C36 C35 C37 110.2(4)
C36 C35 C34 109.7(3)
C37 C35 C34 110.0(3)
C36 C35 C38 108.9(3)
C37 C35 C38 109.3(4)
C34 C35 C38 108.8(3)
N3 B N5 109.5(3)
N3 B N1 110.1(3)
N5 B N1 109.6(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co O 1.859(3)
Co N4 2.033(3)
Co N6 2.046(3)
Co N2 2.051(3)
N1 C12 1.353(4)
N1 N2 1.382(4)
N1 B 1.541(5)
N2 C14 1.335(4)
N3 C22 1.352(4)
N3 N4 1.379(4)
N3 B 1.540(5)
N4 C24 1.341(4)
N5 C32 1.356(4)
N5 N6 1.384(4)
N5 B 1.544(5)
N6 C34 1.340(4)
C11 C12 1.490(5)
C12 C13 1.378(5)
C13 C14 1.399(5)
C14 C15 1.522(5)
C15 C18 1.495(6)
C15 C16 1.524(6)
C15 C17 1.537(6)
C21 C22 1.481(5)
C22 C23 1.385(5)
C23 C24 1.398(5)
C24 C25 1.528(5)
C25 C27 1.520(6)
C25 C26 1.526(6)
C25 C28 1.535(5)
C31 C32 1.486(5)
C32 C33 1.375(5)
C33 C34 1.399(5)
C34 C35 1.526(5)
C35 C36 1.519(5)
C35 C37 1.521(6)
C35 C38 1.531(5)
