#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:17:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179808 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/04/7010483.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_7010483
loop_
_publ_author_name
'Hammes, Brian S.'
'Carrano, Mary W.'
'Carrano, Carl J.'
_publ_section_title
;
 New H-bond accepting tris(pyrazolyl)borates: stabilization of metal
 aquo species as models for the vicinal oxygen chelate enzyme
 superfamily
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1448
_journal_paper_doi               10.1039/b009621k
_journal_year                    2001
_chemical_formula_sum            'C21 H30 B Cl Cu N6 O15'
_chemical_formula_weight         716.31
_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
_cell_angle_alpha                106.982(11)
_cell_angle_beta                 108.75(3)
_cell_angle_gamma                103.97(2)
_cell_formula_units_Z            2
_cell_length_a                   12.106(3)
_cell_length_b                   12.6519(11)
_cell_length_c                   13.012(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.06
_cell_volume                     1676.7(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/ω 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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4402
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.81
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             738
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.131
_refine_ls_goodness_of_fit_obs   1.146
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         4152
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.163
_refine_ls_restrained_S_obs      1.145
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_obs          0.0602
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1141P)²+2.5769P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1979
_refine_ls_wR_factor_obs         0.1766
_reflns_number_observed          3480
_reflns_number_total             4157
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b009621k.txt
_cod_data_source_block           bsh78
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1141P)^2^+2.5769P] 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^)+(0.1141P)^2^+2.5769P] 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        1676.7(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010483
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 0.62995(6) 0.51126(6) 0.72423(5) 0.0426(3) Uani 1 d . .
O1 O 0.7041(4) 0.6605(4) 0.5891(4) 0.0630(12) Uani 1 d . .
O2 O 0.8887(5) 0.8085(5) 0.6546(5) 0.088(2) Uani 1 d . .
O3 O 0.3965(4) 0.5809(4) 0.6382(4) 0.0654(12) Uani 1 d . .
O4 O 0.2745(5) 0.6027(6) 0.7335(4) 0.085(2) Uani 1 d . .
O5 O 0.5271(4) 0.1919(4) 0.6474(4) 0.0670(12) Uani 1 d . .
O6 O 0.6298(4) 0.1025(4) 0.7471(4) 0.0649(12) Uani 1 d . .
O7 O 0.6858(6) 0.4384(5) 0.6026(4) 0.0682(13) Uani 1 d D .
H7 H 0.6886(94) 0.3825(55) 0.5875(87) 0.107(39) Uiso 1 d D .
O8 O 0.4642(4) 0.3790(4) 0.6346(4) 0.0550(11) Uani 1 d D .
H8 H 0.4708(53) 0.3247(47) 0.6243(50) 0.032(18) Uiso 1 d D .
N1 N 0.7882(4) 0.6528(4) 0.8140(4) 0.0445(11) Uani 1 d . .
N2 N 0.8461(4) 0.6907(4) 0.9344(4) 0.0445(11) Uani 1 d . .
N3 N 0.5757(4) 0.5925(4) 0.8440(4) 0.0437(11) Uani 1 d . .
N4 N 0.6490(4) 0.6211(4) 0.9595(4) 0.0430(11) Uani 1 d . .
N5 N 0.6913(4) 0.4118(4) 0.8434(4) 0.0459(11) Uani 1 d . .
N6 N 0.7782(4) 0.4930(4) 0.9530(4) 0.0434(11) Uani 1 d . .
C1 C 1.0261(6) 0.8596(6) 1.1110(6) 0.067(2) Uani 1 d . .
H1A H 0.9976(6) 0.8163(6) 1.1530(6) 0.100 Uiso 1 calc R .
H1B H 1.0211(6) 0.9368(6) 1.1373(6) 0.100 Uiso 1 calc R .
H1C H 1.1115(6) 0.8683(6) 1.1263(6) 0.100 Uiso 1 calc R .
C2 C 0.9450(5) 0.7933(5) 0.9809(5) 0.0471(14) Uani 1 d . .
C3 C 0.9532(6) 0.8239(5) 0.8899(6) 0.056(2) Uani 1 d . .
H3A H 1.0130(6) 0.8899(5) 0.8955(6) 0.067 Uiso 1 calc R .
C4 C 0.8530(5) 0.7351(5) 0.7877(5) 0.0478(14) Uani 1 d . .
C5 C 0.8061(6) 0.7272(6) 0.6656(6) 0.053(2) Uani 1 d . .
C6 C 0.8557(10) 0.8137(12) 0.5365(9) 0.132(5) Uani 1 d . .
H6A H 0.9003(10) 0.7750(12) 0.4981(9) 0.159 Uiso 1 calc R .
H6B H 0.7665(10) 0.7686(12) 0.4886(9) 0.159 Uiso 1 calc R .
C7 C 0.8781(35) 0.9084(17) 0.5379(16) 0.392(26) Uani 1 d . .
H7B H 0.8539(35) 0.9035(17) 0.4583(16) 0.588 Uiso 1 calc R .
H7C H 0.9665(35) 0.9534(17) 0.5831(16) 0.588 Uiso 1 calc R .
H7D H 0.8324(35) 0.9470(17) 0.5736(16) 0.588 Uiso 1 calc R .
C8 C 0.6439(7) 0.6892(7) 1.1578(5) 0.070(2) Uani 1 d . .
H8B H 0.7259(7) 0.6852(7) 1.1834(5) 0.105 Uiso 1 calc R .
H8C H 0.5910(7) 0.6362(7) 1.1774(5) 0.105 Uiso 1 calc R .
H8D H 0.6503(7) 0.7690(7) 1.1968(5) 0.105 Uiso 1 calc R .
C9 C 0.5879(6) 0.6534(5) 1.0257(5) 0.0503(15) Uani 1 d . .
C10 C 0.4741(6) 0.6462(6) 0.9520(5) 0.056(2) Uani 1 d . .
H10A H 0.4117(6) 0.6630(6) 0.9730(5) 0.068 Uiso 1 calc R .
C11 C 0.4710(5) 0.6085(5) 0.8395(5) 0.0456(14) Uani 1 d . .
C12 C 0.3773(6) 0.5951(5) 0.7251(6) 0.054(2) Uani 1 d . .
C13 C 0.1828(10) 0.6080(12) 0.6277(8) 0.126(4) Uani 1 d . .
H13A H 0.2245(10) 0.6693(12) 0.6076(8) 0.151 Uiso 1 calc R .
H13B H 0.1479(10) 0.5324(12) 0.5602(8) 0.151 Uiso 1 calc R .
C14 C 0.0842(9) 0.6342(12) 0.6563(10) 0.122(4) Uani 1 d . .
H14A H 0.0242(9) 0.6379(12) 0.5894(10) 0.184 Uiso 1 calc R .
H14B H 0.1195(9) 0.7093(12) 0.7229(10) 0.184 Uiso 1 calc R .
H14C H 0.0431(9) 0.5728(12) 0.6757(10) 0.184 Uiso 1 calc R .
C15 C 0.9435(7) 0.5064(7) 1.1357(6) 0.069(2) Uani 1 d . .
H15A H 0.9569(7) 0.5895(7) 1.1604(6) 0.103 Uiso 1 calc R .
H15B H 1.0190(7) 0.4952(7) 1.1349(6) 0.103 Uiso 1 calc R .
H15C H 0.9217(7) 0.4778(7) 1.1899(6) 0.103 Uiso 1 calc R .
C16 C 0.8396(5) 0.4392(5) 1.0144(5) 0.0471(14) Uani 1 d . .
C17 C 0.7877(6) 0.3186(6) 0.9433(5) 0.0520(15) Uani 1 d . .
H17A H 0.8090(6) 0.2585(6) 0.9617(5) 0.062 Uiso 1 calc R .
C18 C 0.6964(5) 0.3069(5) 0.8379(5) 0.0449(13) Uani 1 d . .
C19 C 0.6097(6) 0.1973(5) 0.7339(5) 0.0518(15) Uani 1 d . .
C20 C 0.5512(8) -0.0136(6) 0.6493(7) 0.080(2) Uani 1 d . .
H20A H 0.4632(8) -0.0269(6) 0.6294(7) 0.095 Uiso 1 calc R .
H20B H 0.5661(8) -0.0166(6) 0.5798(7) 0.095 Uiso 1 calc R .
C21 C 0.5824(11) -0.1044(7) 0.6859(9) 0.119(4) Uani 1 d . .
H21A H 0.5316(11) -0.1814(7) 0.6226(9) 0.178 Uiso 1 calc R .
H21B H 0.5670(11) -0.1011(7) 0.7544(9) 0.178 Uiso 1 calc R .
H21C H 0.6695(11) -0.0909(7) 0.7049(9) 0.178 Uiso 1 calc R .
B1 B 0.7850(6) 0.6210(6) 0.9955(6) 0.047(2) Uani 1 d . .
H10B H 0.8326(6) 0.6612(6) 1.0818(6) 0.056 Uiso 1 calc R .
Cl1 Cl 0.8441(3) 0.2154(2) 0.5723(2) 0.0931(7) Uani 1 d D 1
O9 O 0.7980(8) 0.1372(7) 0.4586(5) 0.165(3) Uani 1 d D 1
O10 O 0.7515(8) 0.2467(11) 0.5924(10) 0.239(15) Uani 0.553(10) d PD 1
O11 O 0.9373(11) 0.3133(8) 0.5919(9) 0.164(7) Uani 0.553(10) d PD 1
O12 O 0.8896(16) 0.1646(9) 0.6458(7) 0.313(29) Uani 0.553(10) d PD 1
O10' O 0.8480(23) 0.3354(17) 0.6026(21) 0.214(13) Uani 0.553(10) d P 2
O11' O 0.9761(15) 0.2347(16) 0.6339(17) 0.150(8) Uani 0.553(10) d P 2
O12' O 0.7873(25) 0.1611(37) 0.6199(29) 0.270(19) Uani 0.553(10) d P 2
O13 O 0.6554(12) 1.1158(9) 1.0882(14) 0.260(8) Uani 1 d . .
O14 O 0.7397(6) 0.9360(6) 1.0424(10) 0.165(4) Uani 1 d . .
O15 O 0.6614(25) 1.0014(14) 1.1469(20) 0.364(11) 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O8 Cu1 N1 175.2(2) . . ?
O8 Cu1 O7 89.9(2) . . ?
N1 Cu1 O7 93.0(2) . . ?
O8 Cu1 N3 91.7(2) . . ?
N1 Cu1 N3 85.1(2) . . ?
O7 Cu1 N3 176.7(2) . . ?
O8 Cu1 N5 88.7(2) . . ?
N1 Cu1 N5 94.7(2) . . ?
O7 Cu1 N5 96.8(2) . . ?
N3 Cu1 N5 86.1(2) . . ?
C5 O2 C6 117.6(6) . . ?
C12 O4 C13 114.5(6) . . ?
C19 O6 C20 117.7(5) . . ?
C4 N1 N2 105.9(4) . . ?
C4 N1 Cu1 135.2(4) . . ?
N2 N1 Cu1 118.6(3) . . ?
C2 N2 N1 110.1(4) . . ?
C2 N2 B1 130.8(5) . . ?
N1 N2 B1 118.8(4) . . ?
C11 N3 N4 107.1(4) . . ?
C11 N3 Cu1 134.7(4) . . ?
N4 N3 Cu1 116.9(3) . . ?
C9 N4 N3 109.3(5) . . ?
C9 N4 B1 131.0(5) . . ?
N3 N4 B1 119.5(4) . . ?
C18 N5 N6 106.3(4) . . ?
C18 N5 Cu1 142.0(4) . . ?
N6 N5 Cu1 109.0(3) . . ?
C16 N6 N5 110.5(4) . . ?
C16 N6 B1 129.0(5) . . ?
N5 N6 B1 120.1(4) . . ?
N2 C2 C3 108.3(5) . . ?
N2 C2 C1 123.3(5) . . ?
C3 C2 C1 128.4(6) . . ?
C2 C3 C4 105.2(5) . . ?
N1 C4 C3 110.5(5) . . ?
N1 C4 C5 119.3(5) . . ?
C3 C4 C5 129.9(6) . . ?
O1 C5 O2 125.4(6) . . ?
O1 C5 C4 124.1(6) . . ?
O2 C5 C4 110.4(6) . . ?
C7 C6 O2 115.1(14) . . ?
N4 C9 C10 108.0(5) . . ?
N4 C9 C8 122.3(6) . . ?
C10 C9 C8 129.7(6) . . ?
C9 C10 C11 105.5(5) . . ?
N3 C11 C10 110.1(5) . . ?
N3 C11 C12 119.1(5) . . ?
C10 C11 C12 130.6(6) . . ?
O3 C12 O4 125.7(6) . . ?
O3 C12 C11 123.2(6) . . ?
O4 C12 C11 111.1(5) . . ?
C14 C13 O4 108.2(8) . . ?
N6 C16 C17 107.3(5) . . ?
N6 C16 C15 122.6(5) . . ?
C17 C16 C15 130.2(5) . . ?
C16 C17 C18 105.1(5) . . ?
N5 C18 C17 110.8(5) . . ?
N5 C18 C19 121.2(5) . . ?
C17 C18 C19 128.0(5) . . ?
O5 C19 O6 123.5(6) . . ?
O5 C19 C18 125.0(5) . . ?
O6 C19 C18 111.5(5) . . ?
C21 C20 O6 108.4(6) . . ?
N6 B1 N2 111.4(5) . . ?
N6 B1 N4 109.1(5) . . ?
N2 B1 N4 106.3(4) . . ?
O12 Cl1 O10 109.56(10) . . ?
O12 Cl1 O9 109.54(10) . . ?
O10 Cl1 O9 109.44(10) . . ?
O12 Cl1 O11 109.51(10) . . ?
O10 Cl1 O11 109.44(10) . . ?
O9 Cl1 O11 109.34(10) . . ?
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
Cu1 O8 1.981(5) . ?
Cu1 N1 1.981(5) . ?
Cu1 O7 1.986(5) . ?
Cu1 N3 1.991(4) . ?
Cu1 N5 2.322(4) . ?
O1 C5 1.202(7) . ?
O2 C5 1.326(8) . ?
O2 C6 1.485(10) . ?
O3 C12 1.198(7) . ?
O4 C12 1.307(8) . ?
O4 C13 1.496(9) . ?
O5 C19 1.213(7) . ?
O6 C19 1.327(7) . ?
O6 C20 1.462(8) . ?
N1 C4 1.344(7) . ?
N1 N2 1.367(6) . ?
N2 C2 1.345(7) . ?
N2 B1 1.558(8) . ?
N3 C11 1.317(7) . ?
N3 N4 1.359(6) . ?
N4 C9 1.344(7) . ?
N4 B1 1.560(8) . ?
N5 C18 1.326(7) . ?
N5 N6 1.362(6) . ?
N6 C16 1.354(7) . ?
N6 B1 1.523(8) . ?
C1 C2 1.496(8) . ?
C2 C3 1.374(8) . ?
C3 C4 1.391(9) . ?
C4 C5 1.468(8) . ?
C6 C7 1.16(2) . ?
C8 C9 1.505(8) . ?
C9 C10 1.366(9) . ?
C10 C11 1.386(8) . ?
C11 C12 1.485(8) . ?
C13 C14 1.441(13) . ?
C15 C16 1.489(8) . ?
C16 C17 1.385(9) . ?
C17 C18 1.397(8) . ?
C18 C19 1.464(8) . ?
C20 C21 1.450(11) . ?
Cl1 O12 1.350(5) . ?
Cl1 O10 1.351(5) . ?
Cl1 O9 1.352(5) . ?
Cl1 O11 1.352(5) . ?
