#------------------------------------------------------------------------------ #$Date: 2016-01-25 10:24:14 +0000 (Mon, 25 Jan 2016) $ #$Revision: 175013 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100902.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_1100902 loop_ _publ_author_name 'Yamada, Junji' 'Fujiki, Michiya' 'Nomura, Kotohiro' _publ_section_title ; A Vanadium(V) Alkylidene Complex Exhibiting Remarkable Catalytic Activity for Ring-Opening Metathesis Polymerization (ROMP) ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2248 _journal_page_last 2250 _journal_paper_doi 10.1021/om0501834 _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C17 H27 Cl2 N2 V ' _chemical_formula_sum 'C17 H27 Cl2 N2 V' _chemical_formula_weight 381.26 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 101.19(3) _cell_angle_beta 111.44(4) _cell_angle_gamma 101.37(3) _cell_formula_units_Z 2 _cell_length_a 9.814(4) _cell_length_b 9.861(4) _cell_length_c 11.505(5) _cell_measurement_reflns_used 10365 _cell_measurement_temperature 243.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.0 _cell_volume 971.9(7) _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.9966 _diffrn_measured_fraction_theta_max 0.9966 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_limit_h_max 11 _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 -14 _diffrn_reflns_number 9512 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_T_max 0.791 _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 400.00 _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.24 _refine_diff_density_min -0.65 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 295 _refine_ls_number_reflns 3819 _refine_ls_R_factor_gt 0.0360 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 19.2628 0.2819 15.7880 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0450 _reflns_number_gt 3819 _reflns_number_total 4443 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_chemical_formula_sum_orig 'C17 H27 Cl2 N2 V ' _cod_database_code 1100902 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V(1) V 0.95458(3) 0.37802(2) 1.31172(3) 0.03650(7) Uani 1.00 1 d . . . Cl(1) Cl 0.96971(5) 0.60837(4) 1.40645(4) 0.0457(1) Uani 1.00 1 d . . . Cl(2) Cl 1.16963(4) 0.31305(5) 1.35910(4) 0.0469(1) Uani 1.00 1 d . . . N(1) N 0.8963(1) 0.3705(1) 1.1551(1) 0.0395(3) Uani 1.00 1 d . . . N(2) N 0.7968(1) 0.2392(1) 1.2977(1) 0.0353(3) Uani 1.00 1 d . . . C(1) C 0.8506(2) 0.3660(1) 1.0266(2) 0.0398(4) Uani 1.00 1 d . . . C(2) C 0.7643(2) 0.4582(2) 0.9789(2) 0.0462(4) Uani 1.00 1 d . . . C(3) C 0.7238(2) 0.4551(2) 0.8496(2) 0.0582(5) Uani 1.00 1 d . . . C(4) C 0.7647(2) 0.3659(2) 0.7697(2) 0.0610(5) Uani 1.00 1 d . . . C(5) C 0.8471(2) 0.2745(2) 0.8164(2) 0.0555(5) Uani 1.00 1 d . . . C(6) C 0.8913(2) 0.2724(2) 0.9447(2) 0.0455(4) Uani 1.00 1 d . . . C(7) C 0.7224(3) 0.5569(2) 1.0670(2) 0.0623(6) Uani 1.00 1 d . . . C(8) C 0.9817(3) 0.1751(2) 0.9959(2) 0.0579(6) Uani 1.00 1 d . . . C(9) C 0.6912(1) 0.1425(1) 1.2963(1) 0.0329(3) Uani 1.00 1 d . . . C(10) C 0.5483(2) 0.1844(2) 1.2996(1) 0.0404(4) Uani 1.00 1 d . . . C(11) C 0.4874(3) 0.1209(3) 1.3884(2) 0.0586(6) Uani 1.00 1 d . . . C(12) C 0.4232(3) 0.1342(4) 1.1608(2) 0.0763(7) Uani 1.00 1 d . . . C(13) C 0.5873(2) 0.3491(2) 1.3496(3) 0.0573(6) Uani 1.00 1 d . . . C(14) C 0.7154(2) -0.0090(2) 1.2940(2) 0.0441(4) Uani 1.00 1 d . . . C(15) C 0.7738(3) -0.0175(3) 1.4350(3) 0.0689(7) Uani 1.00 1 d . . . C(16) C 0.5716(3) -0.1347(2) 1.2054(3) 0.0739(7) Uani 1.00 1 d . . . C(17) C 0.8386(3) -0.0250(2) 1.2458(3) 0.0635(6) Uani 1.00 1 d . . . H(1) H 0.665(3) 0.521(3) 0.815(2) 0.065(6) Uiso 1.00 1 c . . . H(2) H 0.737(3) 0.362(3) 0.682(3) 0.071(7) Uiso 1.00 1 c . . . H(3) H 0.874(3) 0.212(2) 0.764(2) 0.048(5) Uiso 1.00 1 c . . . H(4) H 0.678(4) 0.618(4) 1.032(4) 0.11(1) Uiso 1.00 1 c . . . H(5) H 0.6531 0.5013 1.0920 0.077 Uiso 1.00 1 c R . . H(6) H 0.8122 0.6136 1.1426 0.077 Uiso 1.00 1 c R . . H(7) H 1.077(3) 0.224(3) 1.058(2) 0.058(6) Uiso 1.00 1 c . . . H(8) H 0.9308 0.1181 1.0340 0.078 Uiso 1.00 1 c R . . H(9) H 0.9918 0.1136 0.9269 0.078 Uiso 1.00 1 c R . . H(10) H 0.461(3) 0.011(3) 1.366(3) 0.086(9) Uiso 1.00 1 c . . . H(11) H 0.399(3) 0.156(3) 1.390(3) 0.076(7) Uiso 1.00 1 c . . . H(12) H 0.568(3) 0.154(3) 1.476(3) 0.070(7) Uiso 1.00 1 c . . . H(13) H 0.334(5) 0.162(4) 1.152(4) 0.11(1) Uiso 1.00 1 c . . . H(14) H 0.378(4) 0.025(3) 1.125(3) 0.081(8) Uiso 1.00 1 c . . . H(15) H 0.465(3) 0.172(3) 1.108(3) 0.074(7) Uiso 1.00 1 c . . . H(16) H 0.619(3) 0.398(2) 1.300(2) 0.054(6) Uiso 1.00 1 c . . . H(17) H 0.497(3) 0.378(3) 1.357(3) 0.072(7) Uiso 1.00 1 c . . . H(18) H 0.672(3) 0.394(3) 1.441(3) 0.074(7) Uiso 1.00 1 c . . . H(19) H 0.801(3) -0.105(3) 1.428(3) 0.082(8) Uiso 1.00 1 c . . . H(20) H 0.695(4) -0.026(3) 1.466(3) 0.091(9) Uiso 1.00 1 c . . . H(21) H 0.876(4) 0.074(4) 1.498(4) 0.11(1) Uiso 1.00 1 c . . . H(22) H 0.484(4) -0.132(3) 1.228(3) 0.089(9) Uiso 1.00 1 c . . . H(23) H 0.598(3) -0.231(3) 1.210(3) 0.084(8) Uiso 1.00 1 c . . . H(24) H 0.526(4) -0.139(4) 1.111(4) 0.10(1) Uiso 1.00 1 c . . . H(25) H 0.936(3) 0.045(3) 1.297(3) 0.069(7) Uiso 1.00 1 c . . . H(26) H 0.815(3) -0.009(3) 1.165(3) 0.061(6) Uiso 1.00 1 c . . . H(27) H 0.853(5) -0.128(4) 1.243(4) 0.12(1) Uiso 1.00 1 c . . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; V V 0.300 0.529 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ;