#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:56:50 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178925 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/54/4115468.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_4115468
loop_
_publ_author_name
'Roger Alberto'
'Kirstin Ortner'
'Nigel Wheatley'
'Roger Schibli'
'August P. Schubiger'
_publ_contact_author_address
'Institute of Inorganic Chemistry, University of Zuerich, CH-8057 Zuerich'
_publ_contact_author_email       ariel@aci.unizh.ch
_publ_contact_author_fax         +41-1-6356803
_publ_contact_author_name        'Roger Alberto'
_publ_contact_author_phone       +41-1-6364631
_publ_section_title
;
 Synthesis and Properties of Boranocarbonate: A Convenient in Situ CO
 Source for the Aqueous Preparation of [99mTc(OH2)3(CO)3]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3135
_journal_page_last               3136
_journal_paper_doi               10.1021/ja003932b
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         'CH3 B O2H, C18 H36 K N2 O6'
_chemical_formula_sum            'C19 H40 B K N2 O8'
_chemical_formula_weight         474.44
_chemical_name_common            '[K(cryptand)]H3BCO2H'
_chemical_name_systematic
;
Potassium (4,7,13,16,21,24-hexaoxa-1,10-diazobicyclo[8.8.8]hexacosane)
boranocarbonate
;
_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                106.269(12)
_cell_angle_beta                 105.153(12)
_cell_angle_gamma                111.573(11)
_cell_formula_units_Z            2
_cell_length_a                   11.1315(11)
_cell_length_b                   11.4183(11)
_cell_length_c                   12.4438(13)
_cell_measurement_reflns_used    196
_cell_measurement_temperature    183(2)
_cell_volume                     1289.0(3)
_computing_cell_refinement       'IPDS (STOE, 1999)'
_computing_data_collection       'IPDS (STOE, 1999)'
_computing_data_reduction        'X-RED (STOE, 1999)'
_computing_molecular_graphics    'Zortep (Zsolnai, 1994), Platon (Spek, 1993)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       '/f oscillation 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0893
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5782
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  7.7
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9520
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0520P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                3003
_reflns_number_total             5782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja003932b.cif
_cod_data_source_block           JA003932B
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1289.0(2)
_cod_database_code               4115468
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_calc_flag
_atom_site_refinement_flags
B1 B 1.2925(4) 1.6553(4) 0.8844(3) 0.0412(7) Uani 1 d .
H1 H 1.239(3) 1.610(3) 0.780(2) 0.046(7) Uiso 1 d .
H2 H 1.363(3) 1.767(3) 0.915(2) 0.056(8) Uiso 1 d .
H3 H 1.207(3) 1.644(3) 0.925(2) 0.051(7) Uiso 1 d .
C1 C 1.3872(2) 1.5890(3) 0.9333(2) 0.0336(5) Uani 1 d .
O1 O 1.41784(19) 1.50744(19) 0.87022(15) 0.0444(5) Uani 1 d .
O2 O 1.4378(2) 1.6239(2) 1.05564(15) 0.0478(5) Uani 1 d .
H4 H 1.485(4) 1.574(4) 1.075(3) 0.075(10) Uiso 1 d .
K1 K 0.83845(6) 0.95871(6) 0.70756(5) 0.03223(14) Uani 1 d .
N1 N 0.8206(2) 1.2231(2) 0.73849(18) 0.0345(5) Uani 1 d .
C2 C 0.6787(3) 1.2011(3) 0.7320(2) 0.0407(6) Uani 1 d .
H2A H 0.6122 1.1579 0.6448 0.049 Uiso 1 calc R
H2B H 0.6842 1.2923 0.7713 0.049 Uiso 1 calc R
C3 C 0.6212(3) 1.1111(3) 0.7930(2) 0.0381(6) Uani 1 d .
H3A H 0.6911 1.1477 0.8780 0.046 Uiso 1 calc R
H3B H 0.5334 1.1110 0.7966 0.046 Uiso 1 calc R
O3 O 0.59216(17) 0.97291(18) 0.72449(14) 0.0362(4) Uani 1 d .
C4 C 0.5174(3) 0.8792(3) 0.7676(2) 0.0380(6) Uani 1 d .
H4A H 0.4221 0.8714 0.7508 0.046 Uiso 1 calc R
H4B H 0.5687 0.9150 0.8574 0.046 Uiso 1 calc R
C5 C 0.5036(3) 0.7387(3) 0.7051(2) 0.0413(6) Uani 1 d .
H5A H 0.4422 0.6713 0.7281 0.050 Uiso 1 calc R
H5B H 0.4597 0.7062 0.6151 0.050 Uiso 1 calc R
O4 O 0.64195(18) 0.74800(18) 0.74187(15) 0.0390(4) Uani 1 d .
C6 C 0.6324(3) 0.6132(3) 0.7064(2) 0.0436(6) Uani 1 d .
H6A H 0.5750 0.5582 0.6171 0.052 Uiso 1 calc R
H6B H 0.5852 0.5642 0.7497 0.052 Uiso 1 calc R
C7 C 0.7792(3) 0.6268(3) 0.7379(3) 0.0446(7) Uani 1 d .
H7A H 0.8347 0.6813 0.8275 0.054 Uiso 1 calc R
H7B H 0.7710 0.5332 0.7173 0.054 Uiso 1 calc R
C8 C 0.8474(3) 1.2626(3) 0.6411(2) 0.0434(6) Uani 1 d .
H8A H 0.9501 1.3024 0.6614 0.052 Uiso 1 calc R
H8B H 0.8208 1.3361 0.6396 0.052 Uiso 1 calc R
C9 C 0.7684(3) 1.1447(3) 0.5145(2) 0.0462(7) Uani 1 d .
H9A H 0.6657 1.1000 0.4947 0.055 Uiso 1 calc R
H9B H 0.7833 1.1810 0.4530 0.055 Uiso 1 calc R
O5 O 0.81791(19) 1.04516(19) 0.51021(14) 0.0436(5) Uani 1 d .
C10 C 0.7382(4) 0.9282(4) 0.3929(2) 0.0600(8) Uani 1 d .
H10A H 0.7413 0.9606 0.3272 0.072 Uiso 1 calc R
H10B H 0.6381 0.8802 0.3806 0.072 Uiso 1 calc R
C11 C 0.7962(4) 0.8310(3) 0.3849(2) 0.0576(8) Uani 1 d .
H11A H 0.7460 0.7551 0.3013 0.069 Uiso 1 calc R
H11B H 0.8978 0.8798 0.4019 0.069 Uiso 1 calc R
O6 O 0.7790(2) 0.7744(2) 0.47360(15) 0.0518(5) Uani 1 d .
C12 C 0.8312(3) 0.6773(3) 0.4643(2) 0.0499(7) Uani 1 d .
H12A H 0.9352 0.7261 0.4917 0.060 Uiso 1 calc R
H12B H 0.7890 0.6093 0.3779 0.060 Uiso 1 calc R
C13 C 0.7942(3) 0.6036(3) 0.5425(2) 0.0448(7) Uani 1 d .
H13A H 0.6900 0.5559 0.5140 0.054 Uiso 1 calc R
H13B H 0.8249 0.5316 0.5304 0.054 Uiso 1 calc R
C14 C 0.9284(3) 1.3314(3) 0.8605(2) 0.0407(6) Uani 1 d .
H14A H 0.8938 1.3151 0.9233 0.049 Uiso 1 calc R
H14B H 0.9392 1.4227 0.8641 0.049 Uiso 1 calc R
C15 C 1.0724(3) 1.3378(3) 0.8926(2) 0.0402(6) Uani 1 d .
H15A H 1.1060 1.3483 0.8280 0.048 Uiso 1 calc R
H15B H 1.1413 1.4192 0.9710 0.048 Uiso 1 calc R
O7 O 1.06327(17) 1.21377(18) 0.90354(14) 0.0371(4) Uani 1 d .
C16 C 1.1989(3) 1.2184(3) 0.9348(2) 0.0398(6) Uani 1 d .
H16A H 1.2687 1.3020 1.0113 0.048 Uiso 1 calc R
H16B H 1.2313 1.2243 0.8687 0.048 Uiso 1 calc R
C17 C 1.1899(3) 1.0916(3) 0.9522(2) 0.0458(7) Uani 1 d .
H17A H 1.2853 1.0991 0.9801 0.055 Uiso 1 calc R
H17B H 1.1535 1.0834 1.0158 0.055 Uiso 1 calc R
O8 O 1.09774(18) 0.97136(19) 0.83927(14) 0.0415(4) Uani 1 d .
C18 C 1.0941(3) 0.8494(3) 0.8522(2) 0.0481(7) Uani 1 d .
H18A H 1.0518 0.8325 0.9106 0.058 Uiso 1 calc R
H18B H 1.1915 0.8624 0.8847 0.058 Uiso 1 calc R
C19 C 1.0070(3) 0.7264(3) 0.7283(2) 0.0485(7) Uani 1 d .
H19A H 1.0506 0.7453 0.6710 0.058 Uiso 1 calc R
H19B H 1.0105 0.6440 0.7370 0.058 Uiso 1 calc R
N2 N 0.8576(2) 0.6938(2) 0.67429(17) 0.0370(5) Uani 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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
O1 C1 O2 116.9(2)
O1 C1 B1 126.7(2)
O2 C1 B1 116.4(2)
O6 K1 O4 92.26(6)
O6 K1 O8 98.28(6)
O4 K1 O8 101.40(5)
O6 K1 O7 139.52(6)
O4 K1 O7 123.73(5)
O8 K1 O7 60.02(5)
O6 K1 O3 112.05(6)
O4 K1 O3 60.69(5)
O8 K1 O3 144.43(5)
O7 K1 O3 102.43(5)
O6 K1 O5 59.96(5)
O4 K1 O5 132.50(6)
O8 K1 O5 119.02(6)
O7 K1 O5 98.87(6)
O3 K1 O5 92.89(5)
O6 K1 N1 119.35(6)
O4 K1 N1 120.09(5)
O8 K1 N1 120.00(6)
O7 K1 N1 61.14(5)
O3 K1 N1 60.50(5)
O5 K1 N1 60.59(5)
O6 K1 N2 60.11(5)
O4 K1 N2 60.46(5)
O8 K1 N2 59.96(6)
O7 K1 N2 118.95(5)
O3 K1 N2 119.97(6)
O5 K1 N2 118.81(5)
N1 K1 N2 179.34(6)
C8 N1 C14 110.8(2)
C8 N1 C2 110.59(19)
C14 N1 C2 108.98(18)
C8 N1 K1 108.69(13)
C14 N1 K1 108.05(14)
C2 N1 K1 109.71(15)
N1 C2 C3 113.4(2)
O3 C3 C2 108.99(18)
C4 O3 C3 111.02(17)
C4 O3 K1 114.07(13)
C3 O3 K1 112.70(13)
O3 C4 C5 110.10(19)
O4 C5 C4 109.2(2)
C6 O4 C5 111.3(2)
C6 O4 K1 120.71(14)
C5 O4 K1 113.12(14)
O4 C6 C7 109.8(2)
N2 C7 C6 114.4(2)
N1 C8 C9 114.5(2)
O5 C9 C8 109.7(2)
C9 O5 C10 110.5(2)
C9 O5 K1 116.38(13)
C10 O5 K1 111.41(17)
O5 C10 C11 110.6(2)
O6 C11 C10 109.1(2)
C12 O6 C11 109.5(2)
C12 O6 K1 118.70(14)
C11 O6 K1 117.31(16)
O6 C12 C13 109.5(2)
N2 C13 C12 114.6(2)
N1 C14 C15 114.48(19)
O7 C15 C14 109.8(2)
C15 O7 C16 110.61(19)
C15 O7 K1 116.20(14)
C16 O7 K1 113.69(14)
O7 C16 C17 110.2(2)
O8 C17 C16 109.9(2)
C17 O8 C18 110.71(18)
C17 O8 K1 115.66(14)
C18 O8 K1 118.57(15)
O8 C18 C19 109.3(2)
N2 C19 C18 114.2(2)
C13 N2 C19 109.72(19)
C13 N2 C7 110.9(2)
C19 N2 C7 110.1(2)
C13 N2 K1 108.88(14)
C19 N2 K1 109.92(15)
C7 N2 K1 107.28(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
B1 C1 1.602(4)
C1 O1 1.251(3)
C1 O2 1.356(3)
K1 O6 2.8069(18)
K1 O4 2.8195(19)
K1 O8 2.8505(17)
K1 O7 2.8570(19)
K1 O3 2.8630(16)
K1 O5 2.8789(18)
K1 N1 3.021(2)
K1 N2 3.031(2)
N1 C8 1.469(3)
N1 C14 1.476(3)
N1 C2 1.481(3)
C2 C3 1.501(4)
C3 O3 1.431(3)
O3 C4 1.424(3)
C4 C5 1.503(4)
C5 O4 1.441(3)
O4 C6 1.431(3)
C6 C7 1.514(4)
C7 N2 1.477(3)
C8 C9 1.510(4)
C9 O5 1.429(3)
O5 C10 1.436(3)
C10 C11 1.469(4)
C11 O6 1.446(3)
O6 C12 1.420(3)
C12 C13 1.495(4)
C13 N2 1.471(3)
C14 C15 1.516(3)
C15 O7 1.429(3)
O7 C16 1.434(3)
C16 C17 1.494(4)
C17 O8 1.429(3)
O8 C18 1.433(3)
C18 C19 1.514(4)
C19 N2 1.475(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H4 O1 0.94(3) 1.79(4) 2.730(2) 173(3) 2_887
