#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:53:24 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195108 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/21/7042187.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_7042187
loop_
_publ_author_name
'Stylianou, M.'
'Hadjiadamou, I.'
'Drouza, C.'
'Hayes, S. C.'
'Lariou, E.'
'Tantis, I.'
'Lianos, P.'
'Tsipis, A. C.'
'Keramidas, A. D.'
_publ_section_title
;
 Synthesis of new photosensitive H2BBQ(2+)[ZnCl4](2-)/[(ZnCl)2(μ-BBH)]
 complexes, through selective oxidation of H2O to H2O2.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3688
_journal_page_last               3699
_journal_paper_doi               10.1039/c6dt04643f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C15 H26.5 Cl2 N3 O6.83'
_chemical_formula_weight         429.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-12-08 deposited with the CCDC.
2017-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                111.192(5)
_cell_angle_beta                 96.107(4)
_cell_angle_gamma                98.791(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6409(4)
_cell_length_b                   10.4155(4)
_cell_length_c                   12.0145(7)
_cell_measurement_reflns_used    3517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.0450
_cell_measurement_theta_min      3.9490
_cell_volume                     980.88(9)
_computing_cell_refinement
;
'Wed Jul 29 17:01:44 2015'
;
_computing_data_collection
;
'Wed Jul 29 17:01:44 2015'
;
_computing_data_reduction
;
'Wed Jul 29 17:01:44 2015'
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.482
_diffrn_reflns_theta_min         4.008
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Wed Jul 29 17:01:44 2015'
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description
;
'Wed Jul 29 17:01:44 2015'
;
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0718
_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)+(0.0952P)²+4.0765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3524
_reflns_number_total             3870
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04643f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7042187--7042190.cif.'
_cod_original_formula_sum        'C15 H26.50 Cl2 N3 O6.83'
_cod_database_code               7042187
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5552(3) 0.4893(3) 0.2173(2) 0.0203(5) Uani 1 1 d . . . . .
C1 C 0.5394(4) 0.5006(4) 0.1186(3) 0.0153(7) Uani 1 1 d . . . . .
N1 N 0.3820(3) 0.6833(3) 0.1925(3) 0.0153(6) Uani 1 1 d . . . . .
N3 N 0.2859(4) 0.5536(3) 0.3426(3) 0.0189(6) Uani 1 1 d . . . . .
C6 C 0.1573(4) 0.9417(3) 0.1515(3) 0.0100(6) Uani 1 1 d . . . . .
H5 H 0.0582 0.8982 0.1578 0.012 Uiso 1 1 calc R U . . .
C4 C 0.2429(4) 0.7396(3) 0.1719(3) 0.0153(7) Uani 1 1 d . . . . .
H7A H 0.1871 0.7523 0.2398 0.018 Uiso 1 1 calc R U . . .
H7B H 0.1719 0.6714 0.0997 0.018 Uiso 1 1 calc R U . . .
C12 C 0.4542(5) 0.7177(4) 0.5181(3) 0.0233(8) Uani 1 1 d . . . . .
H8 H 0.5329 0.7988 0.5568 0.028 Uiso 1 1 calc R U . . .
C3 C 0.6052(4) 0.4132(3) 0.0197(3) 0.0155(7) Uani 1 1 d . . . . .
H10 H 0.6790 0.3629 0.0354 0.019 Uiso 1 1 calc R U . . .
C9 C 0.4454(4) 1.0703(4) 0.1344(3) 0.0211(7) Uani 1 1 d . . . . .
H11 H 0.5444 1.1148 0.1289 0.025 Uiso 1 1 calc R U . . .
C2 C 0.4381(4) 0.5973(3) 0.0956(3) 0.0142(6) Uani 1 1 d . . . . .
C5 C 0.2811(4) 0.8781(3) 0.1565(3) 0.0151(7) Uani 1 1 d . . . . .
N2 N 0.4292(4) 0.9423(4) 0.1486(3) 0.0280(7) Uani 1 1 d . . . . .
C10 C 0.4683(4) 0.7418(4) 0.3172(3) 0.0171(7) Uani 1 1 d . . . . .
H15A H 0.4657 0.8410 0.3533 0.020 Uiso 1 1 calc R U . . .
H15B H 0.5787 0.7342 0.3162 0.020 Uiso 1 1 calc R U . . .
C14 C 0.2704(5) 0.5243(4) 0.5261(4) 0.0278(9) Uani 1 1 d . . . . .
H16 H 0.2260 0.4747 0.5696 0.033 Uiso 1 1 calc R U . . .
C15 C 0.2196(5) 0.4804(4) 0.4038(3) 0.0233(8) Uani 1 1 d . . . . .
H17 H 0.1398 0.4005 0.3633 0.028 Uiso 1 1 calc R U . . .
C11 C 0.4011(4) 0.6692(4) 0.3953(3) 0.0177(7) Uani 1 1 d . . . . .
C8 C 0.3158(5) 1.1316(4) 0.1283(4) 0.0247(8) Uani 1 1 d . . . . .
H21 H 0.3267 1.2166 0.1180 0.030 Uiso 1 1 calc R U . . .
C7 C 0.1706(5) 1.0657(4) 0.1377(4) 0.0242(8) Uani 1 1 d . . . . .
H23 H 0.0821 1.1060 0.1347 0.029 Uiso 1 1 calc R U . . .
C13 C 0.3888(5) 0.6437(4) 0.5835(3) 0.0279(9) Uani 1 1 d . . . . .
H24 H 0.4249 0.6747 0.6664 0.033 Uiso 1 1 calc R U . . .
Cl2 Cl -0.14739(10) 1.24991(10) 0.16945(8) 0.0248(3) Uani 1 1 d . . . . .
Cl1 Cl -0.18107(11) 0.79018(10) 0.15208(9) 0.0285(3) Uani 1 1 d . . . . .
O2W O 0.1354(4) 0.4074(3) 0.1050(2) 0.0308(7) Uani 1 1 d . . . A 1
O1W O -0.1927(5) 1.0846(4) 0.3403(3) 0.0431(8) Uani 1 1 d . . . B 2
O3W O -0.0652(4) 0.6057(4) 0.2932(3) 0.0410(8) Uani 1 1 d . . . C 3
O4W O 0.2608(6) 0.9771(4) 0.4488(3) 0.0488(10) Uani 1 1 d . . . D 4
O6W O 0.1080(5) 1.1975(4) 0.4808(4) 0.0535(10) Uani 1 1 d . . . E 5
O1P O -0.0263(7) 1.0807(6) 0.4975(5) 0.010(2) Uiso 0.348(11) 1 d . . P F 6
O2P O 0.1931(12) 1.0385(12) 0.4412(9) 0.027(4) Uiso 0.290(14) 1 d . . P G 7
O3P O -0.0433(13) 0.6985(12) 0.3661(10) 0.008(4) Uiso 0.191(11) 1 d . . P H 8
H1N H 0.256(5) 0.526(4) 0.272(4) 0.012(10) Uiso 1 1 d . . . . .
H2N H 0.527(5) 0.891(4) 0.152(4) 0.015(10) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
O1 C1 C3 120.8(3) .
O1 C1 C2 120.2(3) .
C3 C1 C2 118.8(3) .
C2 N1 C4 119.9(3) .
C2 N1 C10 123.7(3) .
C4 N1 C10 115.6(3) .
C11 N3 C15 123.2(3) .
C11 N3 H1N 118(3) .
C15 N3 H1N 118(3) .
C7 C6 C5 123.0(3) .
C7 C6 H5 118.5 .
C5 C6 H5 118.5 .
N1 C4 C5 113.7(3) .
N1 C4 H7A 108.8 .
C5 C4 H7A 108.8 .
N1 C4 H7B 108.8 .
C5 C4 H7B 108.8 .
H7A C4 H7B 107.7 .
C11 C12 C13 119.0(4) .
C11 C12 H8 120.5 .
C13 C12 H8 120.5 .
C2 C3 C1 121.5(3) 2_665
C2 C3 H10 119.2 2_665
C1 C3 H10 119.2 .
C8 C9 N2 120.6(3) .
C8 C9 H11 119.7 .
N2 C9 H11 119.7 .
C3 C2 N1 123.0(3) 2_665
C3 C2 C1 119.1(3) 2_665
N1 C2 C1 117.5(3) .
C6 C5 N2 119.1(3) .
C6 C5 C4 115.4(3) .
N2 C5 C4 125.5(3) .
C5 N2 C9 118.7(3) .
C5 N2 H2N 119(2) .
C9 N2 H2N 123(2) .
N1 C10 C11 113.3(3) .
N1 C10 H15A 108.9 .
C11 C10 H15A 108.9 .
N1 C10 H15B 108.9 .
C11 C10 H15B 108.9 .
H15A C10 H15B 107.7 .
C15 C14 C13 118.7(4) .
C15 C14 H16 120.6 .
C13 C14 H16 120.6 .
N3 C15 C14 119.6(4) .
N3 C15 H17 120.2 .
C14 C15 H17 120.2 .
N3 C11 C12 119.0(3) .
N3 C11 C10 118.7(3) .
C12 C11 C10 122.3(3) .
C7 C8 C9 119.2(3) .
C7 C8 H21 120.4 .
C9 C8 H21 120.4 .
C6 C7 C8 119.3(3) .
C6 C7 H23 120.3 .
C8 C7 H23 120.3 .
C14 C13 C12 120.4(4) .
C14 C13 H24 119.8 .
C12 C13 H24 119.8 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.230(4) .
C1 C3 1.443(5) .
C1 C2 1.508(5) .
N1 C2 1.375(4) .
N1 C4 1.451(4) .
N1 C10 1.462(4) .
N3 C11 1.338(5) .
N3 C15 1.345(5) .
N3 H1N 0.79(4) .
C6 C7 1.349(5) .
C6 C5 1.349(5) .
C6 H5 0.9300 .
C4 C5 1.511(4) .
C4 H7A 0.9700 .
C4 H7B 0.9700 .
C12 C11 1.375(5) .
C12 C13 1.390(5) .
C12 H8 0.9300 .
C3 C2 1.355(5) 2_665
C3 H10 0.9300 .
C9 C8 1.379(6) .
C9 N2 1.393(5) .
C9 H11 0.9300 .
C2 C3 1.355(5) 2_665
C5 N2 1.380(5) .
N2 H2N 1.07(4) .
C10 C11 1.511(5) .
C10 H15A 0.9700 .
C10 H15B 0.9700 .
C14 C15 1.370(6) .
C14 C13 1.382(6) .
C14 H16 0.9300 .
C15 H17 0.9300 .
C8 C7 1.372(6) .
C8 H21 0.9300 .
C7 H23 0.9300 .
C13 H24 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
C2 N1 C4 C5 -88.7(4) .
C10 N1 C4 C5 81.8(4) .
O1 C1 C3 C2 166.0(3) 2_665
C2 C1 C3 C2 -8.6(5) 2_665
C4 N1 C2 C3 15.9(5) 2_665
C10 N1 C2 C3 -153.9(3) 2_665
C4 N1 C2 C1 -157.9(3) .
C10 N1 C2 C1 32.3(4) .
O1 C1 C2 C3 -166.2(3) 2_665
C3 C1 C2 C3 8.4(5) 2_665
O1 C1 C2 N1 7.9(5) .
C3 C1 C2 N1 -177.6(3) .
C7 C6 C5 N2 0.7(5) .
C7 C6 C5 C4 -179.8(3) .
N1 C4 C5 C6 -172.5(3) .
N1 C4 C5 N2 6.9(5) .
C6 C5 N2 C9 -0.7(5) .
C4 C5 N2 C9 179.9(3) .
C8 C9 N2 C5 0.0(5) .
C2 N1 C10 C11 -104.5(4) .
C4 N1 C10 C11 85.3(4) .
C11 N3 C15 C14 0.1(6) .
C13 C14 C15 N3 0.2(6) .
C15 N3 C11 C12 -0.8(5) .
C15 N3 C11 C10 179.2(3) .
C13 C12 C11 N3 1.2(6) .
C13 C12 C11 C10 -178.7(3) .
N1 C10 C11 N3 7.1(5) .
N1 C10 C11 C12 -172.9(3) .
N2 C9 C8 C7 0.7(6) .
C5 C6 C7 C8 0.0(6) .
C9 C8 C7 C6 -0.6(6) .
C15 C14 C13 C12 0.3(6) .
C11 C12 C13 C14 -0.9(6) .
