#------------------------------------------------------------------------------
#$Date: 2025-08-21 13:21:36 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301847 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/13/7011396.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_7011396
loop_
_publ_author_name
'Nayan K. Solanki'
'Eric J. L. McInnes'
'David Collison'
'Colin A. Kilner'
'John E. Davies'
'Malcolm A. Halcrow'
_publ_section_title
;
 Copper(II) complexes of 2,6-bis(3-tert-butylpyrazol-1-yl)pyridine
;
_journal_issue                   8
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1625
_journal_page_last               1630
_journal_paper_doi               10.1039/b111210b
_journal_year                    2002
_chemical_formula_moiety         'C38 H50 Cl2 Cu2 N10, 2[B F4]'
_chemical_formula_sum            'C38 H50 B2 Cl2 Cu2 F8 N10'
_chemical_formula_weight         1018.48
_chemical_name_systematic
; 
Dichlorobis[2,6-bis(3-tert-butylpyrazolyl)pyridine]dicopper(II) 
ditetrafluoroborate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.4727(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1630(1)
_cell_length_b                   12.9098(2)
_cell_length_c                   19.5616(3)
_cell_measurement_reflns_used    41554
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.61
_cell_volume                     2313.91(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'Area detector 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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41554
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.8428
_exptl_absorpt_correction_T_min  0.6914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5300
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0647P)²+1.0277P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                4438
_reflns_number_total             5300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111210b.txt
_cod_data_source_block           nks130lt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7011396
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.57509(3) 0.475206(18) 0.405502(12) 0.02484(10) Uani 1 1 d . . .
N2 N 0.4296(2) 0.52226(13) 0.33973(9) 0.0252(4) Uani 1 1 d . . .
C3 C 0.3246(2) 0.45769(17) 0.31894(11) 0.0274(4) Uani 1 1 d . . .
C4 C 0.2025(3) 0.4909(2) 0.28316(11) 0.0329(5) Uani 1 1 d . . .
H4 H 0.1306 0.4449 0.2685 0.039 Uiso 1 1 calc R . .
C5 C 0.1925(2) 0.5963(2) 0.27020(11) 0.0330(5) Uani 1 1 d . . .
H5 H 0.1116 0.6216 0.2466 0.040 Uiso 1 1 calc R B .
C6 C 0.3002(2) 0.66512(18) 0.29155(11) 0.0294(5) Uani 1 1 d . . .
H6 H 0.2935 0.7357 0.2827 0.035 Uiso 1 1 calc R . .
C7 C 0.4176(2) 0.62314(16) 0.32662(10) 0.0241(4) Uani 1 1 d . . .
N8 N 0.3524(2) 0.35511(14) 0.33816(9) 0.0305(4) Uani 1 1 d . B .
N9 N 0.4748(2) 0.33395(13) 0.37723(9) 0.0284(4) Uani 1 1 d . B .
C10 C 0.4812(3) 0.23014(17) 0.38100(12) 0.0338(5) Uani 1 1 d . . .
C11 C 0.3624(3) 0.18623(19) 0.34443(12) 0.0422(6) Uani 1 1 d . . .
H11 H 0.3418 0.1161 0.3393 0.051 Uiso 1 1 calc R . .
C12 C 0.2846(3) 0.2664(2) 0.31832(12) 0.0401(6) Uani 1 1 d . . .
H12 H 0.2004 0.2615 0.2917 0.048 Uiso 1 1 calc R B .
C13 C 0.5976(3) 0.17154(17) 0.42039(12) 0.0375(5) Uani 1 1 d . . .
C14 C 0.5603(3) 0.17468(19) 0.49665(12) 0.0409(6) Uani 1 1 d . . .
H14A H 0.6335 0.1378 0.5222 0.049 Uiso 1 1 calc R B .
H14B H 0.4669 0.1428 0.5036 0.049 Uiso 1 1 calc R . .
H14C H 0.5571 0.2454 0.5118 0.049 Uiso 1 1 calc R . .
C15 C 0.7495(3) 0.21583(18) 0.40716(13) 0.0392(6) Uani 1 1 d . . .
H15A H 0.8208 0.1771 0.4328 0.047 Uiso 1 1 calc R B .
H15B H 0.7525 0.2871 0.4211 0.047 Uiso 1 1 calc R . .
H15C H 0.7708 0.2111 0.3593 0.047 Uiso 1 1 calc R . .
C16 C 0.5959(4) 0.0572(2) 0.39700(15) 0.0501(7) Uani 1 1 d . . .
H16A H 0.6696 0.0193 0.4216 0.060 Uiso 1 1 calc R B .
H16B H 0.6151 0.0537 0.3489 0.060 Uiso 1 1 calc R . .
H16C H 0.5019 0.0276 0.4060 0.060 Uiso 1 1 calc R . .
N17 N 0.53584(18) 0.68003(13) 0.35232(9) 0.0239(4) Uani 1 1 d . A .
N18 N 0.64325(18) 0.62853(13) 0.38909(9) 0.0241(4) Uani 1 1 d . A .
C19 C 0.7491(2) 0.69847(17) 0.39896(10) 0.0259(4) Uani 1 1 d D . .
C20 C 0.7084(2) 0.79404(17) 0.36869(11) 0.0291(4) Uani 1 1 d . A .
H20 H 0.7630 0.8548 0.3685 0.035 Uiso 1 1 calc R . .
C21 C 0.5743(2) 0.77974(16) 0.34003(11) 0.0282(4) Uani 1 1 d . . .
H21 H 0.5193 0.8289 0.3165 0.034 Uiso 1 1 calc R A .
C22A C 0.8907(15) 0.6826(13) 0.4401(8) 0.027(3) Uani 0.50 1 d PD A 1
C23A C 0.855(2) 0.6922(15) 0.5165(6) 0.028(3) Uani 0.50 1 d PD A 1
H23A H 0.9429 0.6832 0.5431 0.034 Uiso 0.50 1 calc PR A 1
H23B H 0.7856 0.6400 0.5288 0.034 Uiso 0.50 1 calc PR A 1
H23C H 0.8150 0.7595 0.5254 0.034 Uiso 0.50 1 calc PR A 1
C24A C 0.9591(17) 0.5789(11) 0.4217(9) 0.028(3) Uani 0.50 1 d PD A 1
H24A H 1.0479 0.5698 0.4474 0.033 Uiso 0.50 1 calc PR A 1
H24B H 0.9801 0.5776 0.3737 0.033 Uiso 0.50 1 calc PR A 1
H24C H 0.8925 0.5240 0.4324 0.033 Uiso 0.50 1 calc PR A 1
C25A C 0.9980(16) 0.7700(14) 0.4206(13) 0.038(3) Uani 0.50 1 d PD A 1
H25A H 1.0875 0.7617 0.4459 0.046 Uiso 0.50 1 calc PR A 1
H25B H 0.9555 0.8360 0.4312 0.046 Uiso 0.50 1 calc PR A 1
H25C H 1.0177 0.7666 0.3725 0.046 Uiso 0.50 1 calc PR A 1
C22B C 0.8911(15) 0.6692(12) 0.4340(8) 0.031(4) Uani 0.50 1 d PD A 2
C23B C 0.868(2) 0.6718(15) 0.5125(6) 0.031(3) Uani 0.50 1 d PD A 2
H23D H 0.9565 0.6523 0.5355 0.037 Uiso 0.50 1 calc PR A 2
H23E H 0.7915 0.6243 0.5245 0.037 Uiso 0.50 1 calc PR A 2
H23F H 0.8405 0.7406 0.5262 0.037 Uiso 0.50 1 calc PR A 2
C24B C 0.9428(16) 0.5621(11) 0.4124(9) 0.029(3) Uani 0.50 1 d PD A 2
H24D H 1.0329 0.5461 0.4354 0.035 Uiso 0.50 1 calc PR A 2
H24E H 0.9577 0.5611 0.3638 0.035 Uiso 0.50 1 calc PR A 2
H24F H 0.8705 0.5115 0.4242 0.035 Uiso 0.50 1 calc PR A 2
C25B C 1.0087(16) 0.7504(14) 0.4162(12) 0.039(3) Uani 0.50 1 d PD A 2
H25D H 1.0995 0.7315 0.4377 0.047 Uiso 0.50 1 calc PR A 2
H25E H 0.9787 0.8172 0.4324 0.047 Uiso 0.50 1 calc PR A 2
H25F H 1.0210 0.7528 0.3676 0.047 Uiso 0.50 1 calc PR A 2
Cl26 Cl 0.66901(5) 0.43846(4) 0.50636(2) 0.02726(13) Uani 1 1 d . . .
B27A B 0.7959(15) 0.4486(12) 0.2561(7) 0.030(3) Uani 0.50 1 d PD B 1
F28A F 0.7588(9) 0.4314(8) 0.3237(4) 0.0380(12) Uani 0.50 1 d PD B 1
F29A F 0.8462(17) 0.5479(9) 0.2463(8) 0.033(2) Uani 0.50 1 d PD B 1
F30A F 0.9022(17) 0.3776(12) 0.2375(9) 0.041(3) Uani 0.50 1 d PD B 1
F31A F 0.6716(8) 0.4307(7) 0.2158(3) 0.0516(15) Uani 0.50 1 d PD B 1
B27B B 0.8015(15) 0.4364(11) 0.2447(7) 0.032(3) Uani 0.50 1 d PD B 2
F28B F 0.7230(10) 0.4329(9) 0.3054(4) 0.076(3) Uani 0.50 1 d PD B 2
F29B F 0.7072(9) 0.4224(7) 0.1892(4) 0.073(2) Uani 0.50 1 d PD B 2
F30B F 0.8674(18) 0.5331(10) 0.2384(9) 0.039(3) Uani 0.50 1 d PD B 2
F31B F 0.9063(16) 0.3597(12) 0.2471(9) 0.0322(19) Uani 0.50 1 d PD B 2
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'
Cu Cu 0.3201 1.2651 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
N2 Cu1 N18 78.90(7) . . ?
N2 Cu1 N9 78.59(7) . . ?
N18 Cu1 N9 154.42(7) . . ?
N2 Cu1 Cl26 157.46(6) . . ?
N18 Cu1 Cl26 103.05(5) . . ?
N9 Cu1 Cl26 102.40(5) . . ?
N2 Cu1 F28A 96.50(16) . . ?
N18 Cu1 F28A 84.8(3) . . ?
N9 Cu1 F28A 85.9(2) . . ?
Cl26 Cu1 F28A 106.03(15) . . ?
N2 Cu1 F28B 85.5(2) . . ?
N18 Cu1 F28B 85.5(3) . . ?
N9 Cu1 F28B 80.8(3) . . ?
Cl26 Cu1 F28B 117.0(2) . . ?
F28A Cu1 F28B 11.4(3) . . ?
N2 Cu1 Cl26 75.96(5) . 3_666 ?
N18 Cu1 Cl26 87.84(5) . 3_666 ?
N9 Cu1 Cl26 98.29(5) . 3_666 ?
Cl26 Cu1 Cl26 81.652(18) . 3_666 ?
F28A Cu1 Cl26 170.4(2) . 3_666 ?
F28B Cu1 Cl26 161.2(2) . 3_666 ?
C7 N2 C3 119.63(19) . . ?
C7 N2 Cu1 119.23(14) . . ?
C3 N2 Cu1 119.73(14) . . ?
N2 C3 C4 122.6(2) . . ?
N2 C3 N8 112.33(19) . . ?
C4 C3 N8 125.1(2) . . ?
C3 C4 C5 116.6(2) . . ?
C4 C5 C6 121.8(2) . . ?
C7 C6 C5 116.5(2) . . ?
N2 C7 C6 122.8(2) . . ?
N2 C7 N17 112.46(18) . . ?
C6 C7 N17 124.76(19) . . ?
C12 N8 N9 111.04(19) . . ?
C12 N8 C3 129.8(2) . . ?
N9 N8 C3 118.80(17) . . ?
C10 N9 N8 105.24(18) . . ?
C10 N9 Cu1 145.86(17) . . ?
N8 N9 Cu1 108.89(12) . . ?
N9 C10 C11 109.8(2) . . ?
N9 C10 C13 123.8(2) . . ?
C11 C10 C13 126.4(2) . . ?
C12 C11 C10 106.5(2) . . ?
C11 C12 N8 107.4(2) . . ?
C10 C13 C15 111.45(19) . . ?
C10 C13 C14 108.7(2) . . ?
C15 C13 C14 111.4(2) . . ?
C10 C13 C16 108.7(2) . . ?
C15 C13 C16 108.3(2) . . ?
C14 C13 C16 108.1(2) . . ?
C21 N17 N18 111.30(17) . . ?
C21 N17 C7 129.49(18) . . ?
N18 N17 C7 118.67(16) . . ?
C19 N18 N17 105.21(16) . . ?
C19 N18 Cu1 146.07(14) . . ?
N17 N18 Cu1 108.71(12) . . ?
N18 C19 C20 109.83(18) . . ?
N18 C19 C22B 121.1(6) . . ?
C20 C19 C22B 129.0(6) . . ?
N18 C19 C22A 126.4(7) . . ?
C20 C19 C22A 123.6(7) . . ?
C22B C19 C22A 7.9(12) . . ?
C21 C20 C19 106.74(19) . . ?
N17 C21 C20 106.91(19) . . ?
C24A C22A C19 110.0(11) . . ?
C24A C22A C23A 113.1(11) . . ?
C19 C22A C23A 108.3(10) . . ?
C24A C22A C25A 108.6(11) . . ?
C19 C22A C25A 108.0(11) . . ?
C23A C22A C25A 108.7(11) . . ?
C19 C22B C24B 111.7(11) . . ?
C19 C22B C25B 109.1(10) . . ?
C24B C22B C25B 109.5(11) . . ?
C19 C22B C23B 108.5(10) . . ?
C24B C22B C23B 109.9(10) . . ?
C25B C22B C23B 108.1(11) . . ?
Cu1 Cl26 Cu1 98.348(15) . 3_666 ?
F29A B27A F28A 111.5(12) . . ?
F29A B27A F30A 110.0(12) . . ?
F28A B27A F30A 108.8(10) . . ?
F29A B27A F31A 110.3(10) . . ?
F28A B27A F31A 107.8(10) . . ?
F30A B27A F31A 108.3(12) . . ?
B27A F28A Cu1 141.1(7) . . ?
F31B B27B F30B 110.1(11) . . ?
F31B B27B F29B 111.1(12) . . ?
F30B B27B F29B 108.3(11) . . ?
F31B B27B F28B 108.2(11) . . ?
F30B B27B F28B 109.3(12) . . ?
F29B B27B F28B 109.8(10) . . ?
B27B F28B Cu1 164.9(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
Cu1 N2 1.9425(18) . ?
Cu1 N18 2.1011(17) . ?
Cu1 N9 2.1134(18) . ?
Cu1 Cl26 2.1978(5) . ?
Cu1 F28A 2.400(9) . ?
Cu1 F28B 2.453(10) . ?
Cu1 Cl26 3.0465(6) 3_666 ?
N2 C7 1.332(3) . ?
N2 C3 1.334(3) . ?
C3 C4 1.383(3) . ?
C3 N8 1.399(3) . ?
C4 C5 1.387(4) . ?
C5 C6 1.389(3) . ?
C6 C7 1.382(3) . ?
C7 N17 1.399(3) . ?
N8 C12 1.358(3) . ?
N8 N9 1.380(3) . ?
N9 C10 1.343(3) . ?
C10 C11 1.416(4) . ?
C10 C13 1.513(4) . ?
C11 C12 1.354(4) . ?
C13 C15 1.529(4) . ?
C13 C14 1.534(3) . ?
C13 C16 1.546(3) . ?
N17 C21 1.357(3) . ?
N17 N18 1.384(2) . ?
N18 C19 1.338(3) . ?
C19 C20 1.417(3) . ?
C19 C22B 1.513(13) . ?
C19 C22A 1.535(13) . ?
C20 C21 1.360(3) . ?
C22A C24A 1.522(13) . ?
C22A C23A 1.537(14) . ?
C22A C25A 1.547(14) . ?
C22B C24B 1.523(14) . ?
C22B C25B 1.544(13) . ?
C22B C23B 1.554(13) . ?
B27A F29A 1.377(13) . ?
B27A F28A 1.386(14) . ?
B27A F30A 1.387(13) . ?
B27A F31A 1.399(12) . ?
B27B F31B 1.379(14) . ?
B27B F30B 1.393(12) . ?
B27B F29B 1.393(13) . ?
B27B F28B 1.394(13) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139154571
