#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4060274.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_4060274 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C24 H45 Br3 O Ni P2 Zn' _chemical_formula_moiety 'C24 H45 Br3 O Ni P2 Zn' _chemical_formula_weight 775.36 _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 8.574(9) _cell_length_b 19.26(4) _cell_length_c 19.15(2) _cell_angle_alpha 90 _cell_angle_beta 98.51(2) _cell_angle_gamma 90 _cell_volume 3127.5(80) _cell_formula_units_Z 4 _cell_measurement_reflns_used 53 _cell_measurement_theta_min 2.1147 _cell_measurement_theta_max 27.8764 _cell_measurement_temperature 173.0 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560.00 _exptl_absorpt_coefficient_mu 5.331 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.4807 _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 9482 _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_theta_max 27.88 _diffrn_measured_fraction_theta_max 0.9854 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.9740 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _reflns_number_total 3790 _reflns_number_gt 4309 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0960 _refine_ls_wR_factor_ref 0.2370 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6480 _refine_ls_number_parameters 297 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1213P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 1.4700 _refine_diff_density_max 1.74 _refine_diff_density_min -1.00 _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 0.3017(2) 0.24359(9) 0.35977(9) 0.0718(6) Uani 1.00 1 d . . . Br(3) Br 0.4824(2) 0.20648(10) 0.18091(9) 0.0726(5) Uani 1.00 1 d . . . Br(4) Br 0.4752(2) 0.05622(8) 0.32250(8) 0.0580(5) Uani 1.00 1 d . . . Zn(1) Zn 0.4704(2) 0.17643(8) 0.29963(9) 0.0465(4) Uani 1.00 1 d . . . Ni(1) Ni 0.5745(2) 0.50735(9) 0.65336(9) 0.0438(5) Uani 1.00 1 d . . . P(6) P 0.3854(4) 0.5218(2) 0.7151(2) 0.0431(9) Uani 1.00 1 d . . . P(7) P 0.4040(5) 0.4284(2) 0.6094(2) 0.0515(10) Uani 1.00 1 d . . . O(1) O 0.6965(13) 0.2065(6) 0.3527(6) 0.062(3) Uani 1.00 1 d . . . C(1) C 0.711(2) 0.5833(10) 0.6965(9) 0.063(5) Uani 1.00 1 d . . . H(1A1) H 0.6596 0.6289 0.7001 0.0760 Uiso 1.00 1 c . . . H(1B1) H 0.7863 0.5711 0.7391 0.0760 Uiso 1.00 1 c . . . C(2) C 0.759(2) 0.5676(12) 0.6305(8) 0.073(6) Uani 1.00 1 d . . . C(3) C 0.799(2) 0.4944(13) 0.6177(8) 0.069(6) Uani 1.00 1 d . . . H(3A1) H 0.8789 0.4766 0.6568 0.0830 Uiso 1.00 1 c . . . C(4) C 0.833(2) 0.474(2) 0.555(2) 0.112(10) Uani 1.00 1 d . . . H(4A1) H 0.8708 0.4286 0.5486 0.1340 Uiso 1.00 1 c . . . C(5) C 0.814(2) 0.520(2) 0.5008(11) 0.128(10) Uani 1.00 1 d . . . H(5A1) H 0.8282 0.5026 0.4557 0.1550 Uiso 1.00 1 c . . . C(6) C 0.777(2) 0.588(2) 0.5051(13) 0.114(9) Uani 1.00 1 d . . . H(6A1) H 0.7769 0.6177 0.4656 0.1350 Uiso 1.00 1 c . . . C(7) C 0.736(2) 0.616(1) 0.5743(10) 0.093(7) Uani 1.00 1 d . . . H(7A1) H 0.6974 0.6618 0.5793 0.1100 Uiso 1.00 1 c . . . C(8) C 0.283(2) 0.6043(7) 0.7098(8) 0.047(4) Uani 1.00 1 d . . . H(8A1) H 0.3582 0.6398 0.7338 0.0570 Uiso 1.00 1 c . . . C(9) C 0.233(3) 0.6284(11) 0.6332(11) 0.086(7) Uani 1.00 1 d . . . H(9A1) H 0.1934 0.6762 0.6331 0.1290 Uiso 1.00 1 c . . . H(9B1) H 0.1495 0.5979 0.6101 0.1290 Uiso 1.00 1 c . . . H(9C1) H 0.3238 0.6266 0.6076 0.1290 Uiso 1.00 1 c . . . C(10) C 0.134(2) 0.6053(7) 0.7464(11) 0.068(5) Uani 1.00 1 d . . . H(10A1) H 0.0723 0.6469 0.7320 0.1020 Uiso 1.00 1 c . . . H(10B1) H 0.1656 0.6055 0.7977 0.1020 Uiso 1.00 1 c . . . H(10C1) H 0.0707 0.5639 0.7326 0.1020 Uiso 1.00 1 c . . . C(11) C 0.420(2) 0.4982(9) 0.8096(8) 0.057(5) Uani 1.00 1 d . . . H(11A1) H 0.3158 0.4962 0.8271 0.0680 Uiso 1.00 1 c . . . C(12) C 0.522(3) 0.5575(12) 0.8504(10) 0.096(7) Uani 1.00 1 d . . . H(12A1) H 0.5624 0.5417 0.8983 0.1440 Uiso 1.00 1 c . . . H(12B1) H 0.4561 0.5988 0.8529 0.1440 Uiso 1.00 1 c . . . H(12C1) H 0.6103 0.5689 0.8254 0.1440 Uiso 1.00 1 c . . . C(13) C 0.497(2) 0.4291(11) 0.8212(12) 0.084(6) Uani 1.00 1 d . . . H(13A1) H 0.5521 0.4262 0.8698 0.1260 Uiso 1.00 1 c . . . H(13B1) H 0.5737 0.4232 0.7883 0.1260 Uiso 1.00 1 c . . . H(13C1) H 0.4174 0.3925 0.8132 0.1260 Uiso 1.00 1 c . . . C(14) C 0.2609(12) 0.4546(6) 0.6648(6) 0.033(3) Uani 1.00 1 d . . . H(14A1) H 0.2331 0.4164 0.6953 0.0400 Uiso 1.00 1 c . . . H(14B1) H 0.1641 0.4742 0.6373 0.0400 Uiso 1.00 1 c . . . C(15) C 0.320(3) 0.439(2) 0.5152(10) 0.104(8) Uani 1.00 1 d . . . H(15A1) H 0.4014 0.4168 0.4900 0.1250 Uiso 1.00 1 c . . . C(16) C 0.314(5) 0.508(2) 0.4890(13) 0.19(1) Uani 1.00 1 d . . . H(16A1) H 0.2827 0.5070 0.4376 0.2890 Uiso 1.00 1 c . . . H(16B1) H 0.4173 0.5296 0.5005 0.2890 Uiso 1.00 1 c . . . H(16C1) H 0.2357 0.5343 0.5106 0.2890 Uiso 1.00 1 c . . . C(17) C 0.173(2) 0.3951(13) 0.4927(11) 0.087(7) Uani 1.00 1 d . . . H(17A1) H 0.1441 0.3978 0.4413 0.1300 Uiso 1.00 1 c . . . H(17B1) H 0.0865 0.4126 0.5157 0.1300 Uiso 1.00 1 c . . . H(17C1) H 0.1955 0.3467 0.5066 0.1300 Uiso 1.00 1 c . . . C(18) C 0.422(4) 0.3311(13) 0.6146(13) 0.121(11) Uani 1.00 1 d . . . H(18A1) H 0.3145 0.3124 0.5976 0.1430 Uiso 1.00 1 c . . . C(19) C 0.464(5) 0.306(2) 0.684(2) 0.20(2) Uani 1.00 1 d . . . H(19A1) H 0.4872 0.2560 0.6828 0.3060 Uiso 1.00 1 c . . . H(19B1) H 0.3753 0.3129 0.7107 0.3060 Uiso 1.00 1 c . . . H(19C1) H 0.5566 0.3306 0.7076 0.3060 Uiso 1.00 1 c . . . C(20) C 0.529(4) 0.307(1) 0.5588(12) 0.124(9) Uani 1.00 1 d . . . H(20A1) H 0.5269 0.2561 0.5553 0.1840 Uiso 1.00 1 c . . . H(20B1) H 0.6378 0.3224 0.5738 0.1840 Uiso 1.00 1 c . . . H(20C1) H 0.4893 0.3271 0.5127 0.1840 Uiso 1.00 1 c . . . C(21) C 0.741(2) 0.1912(10) 0.4276(9) 0.072(6) Uani 1.00 1 d . . . H(21A1) H 0.7752 0.1423 0.4344 0.0870 Uiso 1.00 1 c . . . H(21B1) H 0.6503 0.1990 0.4534 0.0870 Uiso 1.00 1 c . . . C(22) C 0.870(2) 0.2382(13) 0.4531(11) 0.089(7) Uani 1.00 1 d . . . H(22A1) H 0.8708 0.2498 0.5035 0.1070 Uiso 1.00 1 c . . . H(22B1) H 0.9730 0.2179 0.4468 0.1070 Uiso 1.00 1 c . . . C(23) C 0.836(4) 0.296(2) 0.4106(13) 0.120(9) Uani 1.00 1 d . . . H(23A1) H 0.9338 0.3203 0.4028 0.1440 Uiso 1.00 1 c . . . H(23B1) H 0.7685 0.3292 0.4323 0.1440 Uiso 1.00 1 c . . . C(24) C 0.750(3) 0.2680(12) 0.342(2) 0.106(9) Uani 1.00 1 d . . . H(24A1) H 0.6613 0.2992 0.3242 0.1280 Uiso 1.00 1 c . . . H(24B1) H 0.8225 0.2658 0.3067 0.1280 Uiso 1.00 1 c . . .