#------------------------------------------------------------------------------ #$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $ #$Revision: 176429 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100790.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_1100790 loop_ _publ_author_name 'Hidenobu Kajitani' 'Yoshiaki Tanabe' 'Shigeki Kuwata' 'Masakazu Iwasaki' 'Youichi Ishii' _publ_section_title ; Cyanamido-Bridged Diiridium Complex: a Reactive Building Block for Polynuclear Cyanamido Complexes ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2251 _journal_page_last 2254 _journal_paper_doi 10.1021/om048978i _journal_volume 24 _journal_year 2005 _chemical_formula_moiety 'C25 H39 Ir2 N4 P ' _chemical_formula_sum 'C25 H39 Ir2 N4 P' _chemical_formula_weight 811.02 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.199(5) _cell_length_b 13.714(5) _cell_length_c 9.781(3) _cell_measurement_reflns_used 22586 _cell_measurement_temperature 108.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.2 _cell_volume 2575(1) _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.9958 _diffrn_measured_fraction_theta_max 0.9958 _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 0.103 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 24765 _diffrn_reflns_theta_full 27.45 _diffrn_reflns_theta_max 27.45 _exptl_absorpt_coefficient_mu 10.435 _exptl_absorpt_correction_T_max 0.593 _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1544.00 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _refine_diff_density_max 3.60 _refine_diff_density_min -2.21 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 184 _refine_ls_number_reflns 2557 _refine_ls_R_factor_gt 0.0580 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[1.3500\s(Fo^2^) + 0.5000]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0680 _reflns_number_gt 2557 _reflns_number_total 3028 _reflns_threshold_expression F^2^>3.0\s(F^2^) _cod_original_formula_sum 'C25 H39 Ir2 N4 P ' _cod_database_code 1100790 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-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 Ir(1) Ir 0.22217(2) 0.2500 0.03820(4) 0.0080(1) Uani 1.00 2 d S . . Ir(2) Ir 0.06294(2) 0.2500 0.16486(4) 0.0086(1) Uani 1.00 2 d S . . P(1) P 0.1780(2) 0.2500 -0.1769(3) 0.0119(7) Uani 1.00 2 d S . . N(1) N 0.1370(4) 0.1611(5) 0.0944(6) 0.012(2) Uani 1.00 1 d . . . N(2) N 0.1437(4) -0.0171(5) 0.1324(7) 0.019(2) Uani 1.00 1 d . . . C(1) C 0.1404(4) 0.0682(6) 0.1149(7) 0.009(2) Uani 1.00 1 d . . . C(2) C 0.3336(7) 0.2500 -0.015(1) 0.017(3) Uani 1.00 2 d S . . C(3) C 0.3171(4) 0.1658(6) 0.0665(8) 0.015(2) Uani 1.00 1 d . . . C(4) C 0.2956(4) 0.1986(6) 0.2009(8) 0.012(2) Uani 1.00 1 d . . . C(5) C 0.3673(8) 0.25000(1) -0.152(1) 0.026(4) Uani 1.00 2 d S . . C(6) C 0.3268(5) 0.0617(7) 0.0210(8) 0.020(2) Uani 1.00 1 d . . . C(7) C 0.2720(5) 0.1323(6) 0.3161(9) 0.017(2) Uani 1.00 1 d . . . C(8) C 0.0018(4) 0.1963(6) 0.3332(7) 0.010(2) Uani 1.00 1 d . . . C(9) C -0.0306(5) 0.1631(6) 0.2084(8) 0.014(2) Uani 1.00 1 d . . . C(10) C -0.0474(6) 0.2500 0.128(1) 0.016(3) Uani 1.00 2 d S . . C(11) C 0.0313(5) 0.1312(6) 0.4429(7) 0.018(2) Uani 1.00 1 d . . . C(12) C -0.0406(4) 0.0609(6) 0.1676(8) 0.016(2) Uani 1.00 1 d . . . C(13) C -0.0815(8) 0.25000(1) -0.007(1) 0.025(4) Uani 1.00 2 d S . . C(14) C 0.0839(6) 0.25000(1) -0.191(1) 0.023(3) Uani 1.00 2 d S . . C(15) C 0.2034(5) 0.1464(6) -0.279(1) 0.025(2) Uani 1.00 1 d . . . H(1) H 0.3726 0.1844 -0.1826 0.032 Uiso 0.50 1 c R . . H(2) H 0.3400 0.2858 -0.2156 0.032 Uiso 0.50 1 c R . . H(3) H 0.4118 0.2798 -0.1432 0.032 Uiso 0.50 1 c R . . H(4) H 0.3750 0.0507 0.0059 0.024 Uiso 1.00 1 c R . . H(5) H 0.3018 0.0491 -0.0610 0.024 Uiso 1.00 1 c R . . H(6) H 0.3107 0.0192 0.0912 0.024 Uiso 1.00 1 c R . . H(7) H 0.3092 0.0895 0.3396 0.020 Uiso 1.00 1 c R . . H(8) H 0.2327 0.0947 0.2893 0.020 Uiso 1.00 1 c R . . H(9) H 0.2603 0.1716 0.3929 0.020 Uiso 1.00 1 c R . . H(10) H -0.0056 0.0926 0.4785 0.021 Uiso 1.00 1 c R . . H(11) H 0.0505 0.1704 0.5140 0.021 Uiso 1.00 1 c R . . H(12) H 0.0664 0.0894 0.4069 0.021 Uiso 1.00 1 c R . . H(13) H -0.0688 0.0291 0.2340 0.019 Uiso 1.00 1 c R . . H(14) H -0.0630 0.0583 0.0810 0.019 Uiso 1.00 1 c R . . H(15) H 0.0032 0.0288 0.1621 0.019 Uiso 1.00 1 c R . . H(16) H -0.0886 0.3157 -0.0360 0.030 Uiso 0.50 1 c R . . H(17) H -0.0522 0.2172 -0.0704 0.030 Uiso 0.50 1 c R . . H(18) H -0.1250 0.2172 -0.0017 0.029 Uiso 0.50 1 c R . . H(19) H 0.0660 0.3100 -0.1560 0.027 Uiso 0.50 1 c R . . H(20) H 0.0712 0.2500 -0.2842 0.027 Uiso 1.00 2 c R . . H(21) H 0.0653 0.1969 -0.1395 0.027 Uiso 0.50 1 c R . . H(22) H 0.2526 0.1386 -0.2786 0.030 Uiso 1.00 1 c R . . H(23) H 0.1879 0.1559 -0.3705 0.030 Uiso 1.00 1 c R . . H(24) H 0.1822 0.0893 -0.2422 0.030 Uiso 1.00 1 c R . . 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) ; N N 0.006 0.003 ; 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) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ;