#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003775.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003775 loop_ _publ_author_name 'Kawabata, S.' 'Nakata, K.' 'Ichikawa, K.' _publ_section_title ; Benzoato[hydrotris(3-phenylpyrazol-1-yl-N^2^)borato]zinc(II) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1554 _journal_page_last 1556 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C34 H27 B1 N6 O2 Zn1' _chemical_formula_sum 'C34 H27 B N6 O2 Zn' _chemical_formula_weight 627.82 _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_type_scat_source IntTabIV _cell_angle_alpha 104.77(4) _cell_angle_beta 111.99(3) _cell_angle_gamma 73.95(4) _cell_formula_units_Z 2 _cell_length_a 12.884(5) _cell_length_b 13.675(6) _cell_length_c 9.844(6) _cell_measurement_reflns_used 13 _cell_measurement_temperature 293 _cell_measurement_theta_max 22.9 _cell_measurement_theta_min 22.7 _cell_volume 1523.1(14) _diffrn_measurement_device 'Rigaku AFC-7R' _diffrn_measurement_method \w/2\q _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4111 _diffrn_reflns_theta_max 55 _diffrn_standards_decay_% -0.44 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.451 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_type 'empirical (DIFABS; Walker & Stuart, 1983)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.37 _exptl_crystal_description prismatic _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.35 _refine_diff_density_min -0.44 _refine_ls_extinction_coef 8040000.0000 _refine_ls_extinction_method 'Zachariasen Type 2 Gaussian Isotropic (1967)' _refine_ls_goodness_of_fit_obs 2.38 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 398 _refine_ls_number_reflns 2338 _refine_ls_R_factor_obs 0.051 _refine_ls_shift/esd_max 0.01 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.001225F^2^]' _refine_ls_wR_factor_obs 0.083 _reflns_number_observed 2338 _reflns_number_total 3836 _reflns_observed_criterion I>5\s(I) _[local]_cod_data_source_file fg1030.cif _[local]_cod_data_source_block fg1030a _[local]_cod_chemical_formula_sum_orig 'C34 H27 B1 N6 O2 Zn1' _cod_original_cell_volume 1523.0(10) _cod_database_code 2003775 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Zn(1) 0.16370(7) 0.75741(7) 0.20112(10) O(1) 0.3148(4) 0.7590(4) 0.3452(6) O(2) 0.2009(4) 0.7861(4) 0.4785(6) N(1) 0.0552(4) 0.6589(4) 0.1485(6) N(2) -0.0422(5) 0.6859(4) 0.0370(6) N(3) 0.1619(4) 0.7247(4) -0.0184(6) N(4) 0.0523(5) 0.7320(4) -0.1148(6) N(5) 0.0416(5) 0.8883(4) 0.1656(6) N(6) -0.0493(4) 0.8713(4) 0.0404(7) C(1) -0.1187(6) 0.6325(6) 0.0251(8) C(2) -0.0709(6) 0.5690(6) 0.1284(9) C(3) 0.0400(6) 0.5867(5) 0.2055(8) C(4) 0.1324(6) .5343(5) 0.3181(9) C(5) 0.1082(5) 0.4858(6) 0.4070(10) C(6) 0.1940(10) 0.4308(7) 0.5070(10) C(7) 0.3030(10) 0.4238(7) 0.5230(10) C(8) 0.3303(8) 0.4703(7) 0.4370(10) C(9) 0.2453(7) 0.5253(6) 0.3330(10) C(10) 0.0530(6) 0.7092(5) -0.2524(8) C(11) 0.1633(7) 0.6856(5) -0.2493(8) C(12) 0.2299(6) 0.6962(5) -0.1016(8) C(13) 0.3549(6) 0.6800(5) -0.0420(9) C(14) 0.4225(8) 0.6124(7) -0.1180(10) C(15) 0.5410(10) 0.6000(9) -0.059(2) C(16) 0.5914(9) 0.6540(10) 0.0740(10) C(17) 0.5262(8) 0.7230(10) 0.1540(10) C(18) 0.4092(6) 0.7359(7) 0.0943(9) C(19) -0.1307(6) 0.9573(6) 0.0283(10) C(20) -0.0924(6) 1.0329(5) 0.1480(10) C(21) 0.0157(6) 0.9871(5) 0.2306(8) C(22) 0.0932(6) 1.0343(5) 0.3688(8) C(23) 0.0481(7) 1.0994(6) 0.4767(9) C(24) 0.1180(10) 1.1455(7) 0.6070(10) C(25) 0.2320(10) 1.1272(8) 0.6320(10) C(26) 0.2783(6) 1.0633(7) 0.5270(10) C(27) 0.2088(7) 1.0179(6) 0.3956(9) C(28) 0.2967(6) 0.7835(5) 0.4716(9) C(29) 0.3927(6) 0.8094(5) 0.6032(8) C(30) 0.4986(7) 0.8016(7) 0.5928(10) C(31) 0.5875(8) 0.8280(10) 0.7190(10) C(32) 0.5727(10) 0.8635(9) 0.8530(10) C(33) 0.4680(10) 0.8726(8) 0.8630(10) C(34) 0.3784(7) 0.8463(7) 0.7405(10) B(1) -0.0521(6) 0.7643(7) -0.0580(10) H1B -0.13204 0.76467 -0.14186 H1 -0.19571 0.63744 -0.04328 H2 -0.10649 0.52124 0.14693 H5 0.02785 0.48855 0.39376 H6 0.17678 0.40106 0.57080 H7 0.36314 0.38647 0.59670 H8 0.41040 0.46375 0.44556 H9 0.26244 0.55755 0.27015 H10 -0.01167 0.71029 -0.34364 H11 0.18917 0.66599 -0.33594 H14 0.39138 0.57168 -0.21173 H15 0.59233 0.55264 -0.10663 H16 0.67422 0.65461 0.11797 H17 0.56221 0.76379 0.24487 H18 0.36233 0.78422 0.15153 H19 -0.20537 0.96573 -0.04732 H20 -0.13212 1.10104 0.17072 H23 -0.03355 1.11311 0.45718 H24 0.08696 1.19232 0.68113 H25 0.27773 1.15941 0.72540 H26 0.36228 1.05178 0.55044 H27 0.24243 0.97263 0.32355 H30 0.51006 0.77789 0.49702 H31 0.66248 0.82418 0.71163 H32 0.63425 0.87822 0.93986 H33 0.45843 0.90134 0.96118 H34 0.30271 0.85426 0.75209 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Zn(1) N(1) 131.3(2) yes O(1) Zn(1) N(3) 113.4(2) yes O(1) Zn(1) N(5) 122.6(2) yes N(1) Zn(1) N(3) 90.0(2) yes N(1) Zn(1) N(5) 97.0(2) yes N(3) Zn(1) N(5) 92.1(2) yes Zn(1) O(1) C(28) 103.5(4) yes O(1) C(28) O(2) 120.9(7) yes O(1) C(28) C(29) 116.6(6) yes O(2) C(28) C(29) 122.5(7) yes O(1) Zn(1) B(1) 169.5(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Zn(1) O(1) 1.935(5) yes Zn(1) N(1) 2.044(6) yes Zn(1) N(3) 2.084(5) yes Zn(1) N(5) 2.038(5) yes O(1) C(28) 1.295(9) yes O(2) C(28) 1.252(8) yes C(28) C(29) 1.463(10) yes Zn(1) O(2) 2.534(6) yes Zn(1) B(1) 2.985(7) yes O(1) B(1) 4.901(8) yes N(1) N(2) 1.355(7) no N(2) C(1) 1.337(9) no N(3) N(4) 1.368(7) no N(4) C(10) 1.313(9) no N(5) N(6) 1.367(8) no N(6) C(19) 1.339(9) no C(1) C(2) 1.360(10) no C(3) C(4) 1.450(10) no C(4) C(9) 1.380(10) no C(6) C(7) 1.340(10) no C(8) C(9) 1.380(10) no C(11) C(12) 1.378(10) no C(13) C(14) 1.370(10) no C(14) C(15) 1.390(10) no C(16) C(17) 1.37(2) no C(19) C(20) 1.390(10) no C(21) C(22) 1.468(10) no C(22) C(27) 1.380(10) no C(24) C(25) 1.370(10) no C(26) C(27) 1.380(10) no C(29) C(30) 1.380(10) no N(1) C(3) 1.341(9) no N(2) B(1) 1.540(10) no N(3) C(12) 1.333(8) no N(4) B(1) 1.557(10) no N(5) C(21) 1.347(8) no N(6) B(1) 1.537(10) no C(2) C(3) 1.401(10) no C(4) C(5) 1.380(10) no C(5) C(6) 1.370(10) no C(7) C(8) 1.360(10) no C(10) C(11) 1.360(10) no C(12) C(13) 1.466(10) no C(13) C(18) 1.390(10) no C(15) C(16) 1.35(2) no C(17) C(18) 1.380(10) no C(20) C(21) 1.390(10) no C(22) C(23) 1.400(10) no C(23) C(24) 1.370(10) no C(25) C(26) 1.370(10) no C(29) C(34) 1.380(10) no C(30) C(31) 1.380(10) no C(32) C(33) 1.360(10) no C(31) C(32) 1.36(2) no C(33) C(34) 1.370(10) no