#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4060273.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_4060273 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C25 H47 Br3 Ni O P2 Zn' _[local]_cod_chemical_formula_sum_orig 'C25 H47 Br3 O Ni P2 Zn' _chemical_formula_moiety 'C25 H47 Br3 O Ni P2 Zn' _chemical_formula_weight 789.39 _symmetry_cell_setting monoclinic _space_group_IT_number 9 _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _[local]_cod_cif_authors_sg_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x+1/2,y+1/2,z' 'x,-y,z+1/2' 'x+1/2,-y+1/2,z+1/2' _cell_length_a 8.315(10) _cell_length_b 18.69(2) _cell_length_c 20.68(2) _cell_angle_alpha 90 _cell_angle_beta 96.90(5) _cell_angle_gamma 90 _cell_volume 3190.5(60) _cell_formula_units_Z 4 _cell_measurement_reflns_used 58 _cell_measurement_theta_min 2.1804 _cell_measurement_theta_max 34.9698 _cell_measurement_temperature 173.0 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592.00 _exptl_absorpt_coefficient_mu 5.227 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6787 _exptl_absorpt_correction_T_max 1.0000 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 10185 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 28.00 _diffrn_measured_fraction_theta_max 0.9718 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.9718 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 32 _reflns_number_total 6198 _reflns_number_gt 5086 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1240 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5975 _refine_ls_number_parameters 306 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.96 _refine_diff_density_min -0.75 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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) ; 'Br' 'Br' -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Ni' 'Ni' 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Zn' 'Zn' 0.284 1.430 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 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 Br(1) Br 0.38564(12) 0.80132(5) 0.37214(6) 0.0479(3) Uani 1.00 1 d . . . Br(2) Br 0.43299(10) 0.95336(5) 0.50922(5) 0.0400(3) Uani 1.00 1 d . . . Br(3) Br 0.26734(13) 0.76176(6) 0.54948(6) 0.0559(4) Uani 1.00 1 d . . . Zn(1) Zn 0.41633(10) 0.83120(5) 0.48379(5) 0.0266(3) Uani 1.00 1 d . . . Ni(1) Ni 0.49797(10) 0.49076(5) 0.31674(5) 0.0175(3) Uani 1.00 1 d . . . P(1) P 0.3252(2) 0.42217(10) 0.25705(11) 0.0173(5) Uani 1.00 1 d . . . P(2) P 0.3231(2) 0.51357(10) 0.38245(10) 0.0165(5) Uani 1.00 1 d . . . O(1) O 0.6516(7) 0.7943(3) 0.5145(3) 0.032(2) Uani 1.00 1 d . . . C(1) C 0.6666(9) 0.5520(5) 0.3650(5) 0.031(3) Uani 1.00 1 d . . . H(1A1) H 0.6311 0.5998 0.3784 0.0370 Uiso 1.00 1 c . . . H(1B1) H 0.7423 0.5280 0.3988 0.0370 Uiso 1.00 1 c . . . C(2) C 0.7032(9) 0.5455(5) 0.2980(4) 0.030(3) Uani 1.00 1 d . . . C(3) C 0.7145(9) 0.4756(5) 0.2734(5) 0.033(3) Uani 1.00 1 d . . . H(3A1) H 0.7949 0.4462 0.3018 0.0390 Uiso 1.00 1 c . . . C(4) C 0.7366(10) 0.4685(8) 0.2058(6) 0.059(4) Uani 1.00 1 d . . . H(4A1) H 0.7518 0.4224 0.1883 0.0710 Uiso 1.00 1 c . . . C(5) C 0.7360(12) 0.5275(9) 0.1662(6) 0.062(4) Uani 1.00 1 d . . . H(5A1) H 0.7520 0.5219 0.1218 0.0750 Uiso 1.00 1 c . . . C(6) C 0.7127(13) 0.5937(9) 0.1902(7) 0.071(5) Uani 1.00 1 d . . . H(6A1) H 0.7092 0.6337 0.1617 0.0850 Uiso 1.00 1 c . . . C(7) C 0.6941(11) 0.6049(6) 0.2540(6) 0.047(3) Uani 1.00 1 d . . . H(7A1) H 0.6752 0.6518 0.2691 0.0560 Uiso 1.00 1 c . . . C(8) C 0.2910(10) 0.4415(5) 0.1693(4) 0.027(2) Uani 1.00 1 d . . . H(8A1) H 0.3895 0.4248 0.1503 0.0320 Uiso 1.00 1 c . . . C(9) C 0.1460(10) 0.4018(5) 0.1333(5) 0.033(3) Uani 1.00 1 d . . . H(9A1) H 0.1325 0.4158 0.0873 0.0490 Uiso 1.00 1 c . . . H(9B1) H 0.0478 0.4140 0.1528 0.0490 Uiso 1.00 1 c . . . H(9C1) H 0.1648 0.3501 0.1367 0.0490 Uiso 1.00 1 c . . . C(10) C 0.2777(11) 0.5223(4) 0.1574(5) 0.033(3) Uani 1.00 1 d . . . H(10A1) H 0.2807 0.5321 0.1110 0.0500 Uiso 1.00 1 c . . . H(10B1) H 0.3685 0.5465 0.1830 0.0500 Uiso 1.00 1 c . . . H(10C1) H 0.1754 0.5398 0.1706 0.0500 Uiso 1.00 1 c . . . C(11) C 0.3530(10) 0.3235(4) 0.2606(5) 0.030(3) Uani 1.00 1 d . . . H(11A1) H 0.2523 0.3014 0.2377 0.0360 Uiso 1.00 1 c . . . C(12) C 0.4927(13) 0.2993(5) 0.2254(5) 0.040(3) Uani 1.00 1 d . . . H(12A1) H 0.4926 0.2469 0.2225 0.0600 Uiso 1.00 1 c . . . H(12B1) H 0.5950 0.3154 0.2495 0.0600 Uiso 1.00 1 c . . . H(12C1) H 0.4812 0.3197 0.1815 0.0600 Uiso 1.00 1 c . . . C(13) C 0.3705(12) 0.2972(5) 0.3300(5) 0.042(3) Uani 1.00 1 d . . . H(13A1) H 0.3781 0.2449 0.3304 0.0630 Uiso 1.00 1 c . . . H(13B1) H 0.2760 0.3121 0.3507 0.0630 Uiso 1.00 1 c . . . H(13C1) H 0.4689 0.3175 0.3539 0.0630 Uiso 1.00 1 c . . . C(14) C 0.1267(9) 0.4381(4) 0.2862(4) 0.020(2) Uani 1.00 1 d . . . H(14A1) H 0.0706 0.4777 0.2609 0.0250 Uiso 1.00 1 c . . . H(14B1) H 0.0590 0.3946 0.2788 0.0250 Uiso 1.00 1 c . . . C(15) C 0.1453(9) 0.4571(4) 0.3586(4) 0.017(2) Uani 1.00 1 d . . . H(15A1) H 0.1550 0.4125 0.3846 0.0210 Uiso 1.00 1 c . . . H(15B1) H 0.0468 0.4826 0.3686 0.0210 Uiso 1.00 1 c . . . C(16) C 0.3722(9) 0.4941(4) 0.4685(4) 0.022(2) Uani 1.00 1 d . . . H(16A1) H 0.2675 0.4923 0.4878 0.0260 Uiso 1.00 1 c . . . C(17) C 0.4524(10) 0.4197(5) 0.4796(5) 0.032(3) Uani 1.00 1 d . . . H(17A1) H 0.4797 0.4113 0.5264 0.0480 Uiso 1.00 1 c . . . H(17B1) H 0.5514 0.4180 0.4582 0.0480 Uiso 1.00 1 c . . . H(17C1) H 0.3771 0.3826 0.4611 0.0480 Uiso 1.00 1 c . . . C(18) C 0.4776(9) 0.5497(5) 0.5066(4) 0.027(2) Uani 1.00 1 d . . . H(18A1) H 0.5044 0.5335 0.5517 0.0410 Uiso 1.00 1 c . . . H(18B1) H 0.4190 0.5952 0.5061 0.0410 Uiso 1.00 1 c . . . H(18C1) H 0.5776 0.5563 0.4866 0.0410 Uiso 1.00 1 c . . . C(19) C 0.2486(10) 0.6051(4) 0.3771(4) 0.025(2) Uani 1.00 1 d . . . H(19A1) H 0.3420 0.6356 0.3952 0.0290 Uiso 1.00 1 c . . . C(20) C 0.2061(13) 0.6290(5) 0.3068(5) 0.040(3) Uani 1.00 1 d . . . H(20A1) H 0.1795 0.6801 0.3057 0.0600 Uiso 1.00 1 c . . . H(20B1) H 0.1127 0.6016 0.2867 0.0600 Uiso 1.00 1 c . . . H(20C1) H 0.2989 0.6206 0.2827 0.0600 Uiso 1.00 1 c . . . C(21) C 0.1138(10) 0.6217(5) 0.4177(5) 0.035(3) Uani 1.00 1 d . . . H(21A1) H 0.0843 0.6723 0.4128 0.0520 Uiso 1.00 1 c . . . H(21B1) H 0.1504 0.6115 0.4636 0.0520 Uiso 1.00 1 c . . . H(21C1) H 0.0193 0.5920 0.4030 0.0520 Uiso 1.00 1 c . . . C(22) C 0.709(1) 0.7274(5) 0.4918(6) 0.055(4) Uani 1.00 1 d . . . H(22A1) H 0.7908 0.7354 0.4613 0.0660 Uiso 1.00 1 c . . . H(22B1) H 0.6191 0.6987 0.4696 0.0660 Uiso 1.00 1 c . . . C(23) C 0.785(2) 0.6906(6) 0.5535(10) 0.116(6) Uani 1.00 1 d . . . H(23A1) H 0.7104 0.6536 0.5668 0.1370 Uiso 1.00 1 c . . . H(23B1) H 0.8874 0.6669 0.5455 0.1370 Uiso 1.00 1 c . . . C(24) C 0.816(2) 0.7411(8) 0.6024(7) 0.085(6) Uani 1.00 1 d . . . H(24A1) H 0.9305 0.7565 0.6064 0.1020 Uiso 1.00 1 c . . . H(24B1) H 0.7929 0.7212 0.6447 0.1020 Uiso 1.00 1 c . . . C(25) C 0.7110(13) 0.7994(6) 0.5837(6) 0.049(3) Uani 1.00 1 d . . . H(25A1) H 0.7701 0.8451 0.5924 0.0590 Uiso 1.00 1 c . . . H(25B1) H 0.6184 0.7989 0.6096 0.0590 Uiso 1.00 1 c . . . _cod_database_code 4060273