#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/01/2010183.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_2010183 loop_ _publ_author_name 'Cotton, F.A.' 'Wojtczak, W.A.' _publ_section_title ; Two zirconium(IV) complexes, [Zr~2~Cl~8~(PMe~3~)~4~] and trans-[ZrI~4~(PMe~2~Ph)~2~] ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1662 _journal_page_last 1664 _journal_paper_doi 10.1107/S0108270194003963 _journal_volume 50 _journal_year 1994 _chemical_formula_sum 'C12 H36 Cl8 P4 Zr2' _chemical_formula_weight 770.4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 93.400(10) _cell_angle_gamma 90. _cell_formula_units_Z 2 _cell_length_a 8.2200(10) _cell_length_b 16.579(2) _cell_length_c 11.1920(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294 _cell_measurement_theta_max 16 _cell_measurement_theta_min 13 _cell_volume 1522.6(3) _diffrn_measurement_device 'Syntex P3/F' _diffrn_measurement_method \w-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 1892 _diffrn_reflns_theta_max 23 _diffrn_standards_decay_% '-36.4% overall' _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.594 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_type 'psi scans at chi = 90\%' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.680 _exptl_crystal_description block _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.309 _refine_diff_density_min -0.312 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 0.801 _refine_ls_number_parameters 172 _refine_ls_number_reflns 1395 _refine_ls_R_factor_obs 0.0288 _refine_ls_shift/esd_max 0.02 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\s^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0376 _reflns_number_observed 1395 _reflns_number_total 1640 _reflns_observed_criterion F~o~^2^>3\s(F~o~^2^) _cod_data_source_file hr1002.cif _cod_data_source_block hr1002_structure_1_of_2 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/\s^2^' 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^'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2010183 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Zr .03610(7) .09081(3) .13616(4) Cl(1) .1338(2) -.05301(9) .06700(10) Cl(2) .1697(2) .04300(10) .32280(10) Cl(3) -.1827(2) .18930(9) .13970(10) Cl(4) .2346(2) .14240(10) .00330(10) P(1) .1686(2) .22560(10) .24770(10) P(2) -.2130(2) .00990(10) .24930(10) C(10) .0698(9) .2524(5) .3822(6) C(11) .3831(8) .2198(5) .2962(7) C(12) .1580(10) .3168(4) .1587(7) C(20) -.4153(8) .0047(5) .1742(6) C(21) -.2515(9) .0649(5) .3854(6) C(22) -.1719(9) -.0909(4) .3048(6) H(10) .090(10) .207(5) .439(7) H(11) -.050(10) .269(5) .367(7) H(12) .110(10) .301(5) .421(7) H(13) .410(10) .178(5) .353(7) H(14) .410(10) .267(5) .328(7) H(15) .430(10) .218(5) .227(7) H(16) .060(10) .325(6) .130(8) H(17) .190(10) .361(5) .208(8) H(18) .190(10) .309(5) .090(8) H(20) -.440(10) .052(5) .139(7) H(21) -.400(10) -.027(5) .104(7) H(22) -.470(10) -.017(5) .234(7) H(23) -.330(10) .045(5) .421(7) H(24) -.160(10) .061(5) .431(7) H(25) -.280(10) .114(5) .364(7) H(26) -.250(10) -.101(5) .343(7) H(27) -.160(10) -.126(5) .245(7) H(28) -.100(10) -.092(5) .356(7) 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 Cl(1) Zr Cl(1)' 72.06(5) yes Cl(1) Zr Cl(2) 80.11(5) yes Cl(1) Zr Cl(3) 147.94(5) yes Cl(1) Zr Cl(4) 84.93(5) yes Cl(1) Zr P(1) 138.18(5) yes Cl(1) Zr P(2) 86.75(5) yes Cl(1)' Zr Cl(2) 147.19(5) yes Cl(1)' Zr Cl(3) 79.73(5) yes Cl(1)' Zr Cl(4) 84.13(5) yes Cl(1)' Zr P(1) 138.53(5) yes Cl(1)' Zr P(2) 85.04(5) yes Cl(2) Zr Cl(3) 120.08(6) yes Cl(2) Zr Cl(4) 110.78(6) yes Cl(2) Zr P(1) 74.27(5) yes Cl(2) Zr P(2) 76.22(5) yes Cl(3) Zr Cl(4) 107.37(6) yes Cl(3) Zr P(1) 73.79(5) yes Cl(3) Zr P(2) 75.74(5) yes Cl(4) Zr P(1) 74.31(5) yes Cl(4) Zr P(2) 167.96(5) yes P(1) Zr P(2) 117.55(5) yes Zr Cl(1) Zr' 107.94(5) yes Zr P(1) C(12) 115.0(2) no C(10) P(1) C(11) 103.9(3) no C(10) P(1) C(12) 104.0(4) no C(11) P(1) C(12) 103.0(4) no Zr P(2) C(20) 119.0(2) no Zr P(2) C(21) 107.8(3) no Zr P(2) C(22) 118.0(2) no C(20) P(2) C(21) 102.2(3) no C(20) P(2) C(22) 105.2(3) no C(21) P(2) C(22) 102.3(3) no Zr P(1) C(10) 113.1(2) no Zr P(1) C(11) 116.4(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Zr Cl(1) 2.646(2) yes Zr Cl(1)' 2.6710(10) yes Zr Cl(2) 2.434(2) yes Zr Cl(3) 2.431(2) yes Zr Cl(4) 2.427(2) yes Zr P(1) 2.752(2) yes Zr P(2) 2.811(2) yes P(1) C(10) 1.808(7) no P(1) C(11) 1.816(7) no P(1) C(12) 1.810(7) no P(2) C(20) 1.820(7) no P(2) C(21) 1.820(7) no P(2) C(22) 1.808(7) no C(10) H(10) 1.00(8) no C(10) H(11) 1.04(8) no C(10) H(12) 0.96(8) no C(11) H(13) 0.96(9) no C(11) H(14) 0.88(9) no C(11) H(15) 0.88(9) no C(12) H(16) 0.87(8) no C(12) H(17) 0.95(9) no C(12) H(18) 0.84(9) no C(20) H(20) 0.89(8) no C(20) H(21) 0.96(8) no C(20) H(22) 0.89(8) no C(21) H(23) 0.88(8) no C(21) H(24) 0.92(8) no C(21) H(25) 0.87(8) no C(22) H(26) 0.83(8) no C(22) H(27) 0.90(8) no C(22) H(28) 0.79(8) no