#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003318.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_2003318 loop_ _publ_author_name 'VanderLende, D. D.' 'Boncella, J. M.' 'Abboud, K. A.' _publ_section_title ; trans-[Ni(Me~3~Ph)(NHPh)(PMe~3~)~2~], a Monomeric Ni^II^--Amide Complex ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 591 _journal_page_last 593 _journal_paper_doi 10.1107/S0108270194011534 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C21 H35 N1 Ni1 P2' _chemical_formula_sum 'C21 H35 N Ni P2' _chemical_formula_weight 422.15 _space_group_IT_number 14 _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 109.72(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.491(1) _cell_length_b 12.368(1) _cell_length_c 15.655(1) _cell_measurement_reflns_used 32 _cell_measurement_temperature 293 _cell_measurement_theta_max 11 _cell_measurement_theta_min 10 _cell_volume 2276.7(3) _diffrn_measurement_device 'Siemens P3m/V' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0125 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 5780 _diffrn_reflns_theta_max 27.5 _diffrn_standards_decay_% 3 _diffrn_standards_interval_count 100 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 1.00 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_type analytical _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.232 _exptl_crystal_description plates _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _refine_diff_density_max -0.29 _refine_diff_density_min -0.30 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.36 _refine_ls_number_parameters 258 _refine_ls_number_reflns 3285 _refine_ls_R_factor_obs 0.0445 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0478 _reflns_number_observed 3285 _reflns_number_total 5248 _reflns_observed_criterion F>6\s(F) _cod_data_source_file bk1063.cif _cod_data_source_block bk1063a _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F) + 0.0004F^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^(F) + 0.0004F^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_original_formula_sum 'C21 H35 N1 Ni1 P2' _cod_database_code 2003318 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ni .46691(4) .15944(3) .16912(3) .0384(2) P1 .65065(8) .14007(8) .23537(7) .0511(4) P2 .28275(8) .17495(8) .10725(6) .0495(4) N .4715(3) .1380(3) .0482(2) .0482(14) C1 .4507(3) .1837(3) .2846(2) .0402(13) C2 .4276(3) .0982(3) .3355(2) .0473(14) C2' .4185(4) -.0153(3) .2998(3) .064(2) C3 .4055(3) .1182(4) .4154(3) .054(2) C4 .4023(3) .2216(3) .4474(2) .054(2) C4' .3693(4) .2435(4) .5302(3) .076(2) C5 .4257(3) .3053(3) .3986(3) .053(2) C6 .4493(3) .2886(3) .3186(2) .0443(13) C6' .4662(4) .3868(3) .2671(3) .063(2) C7 .5083(3) .2050(3) -.0045(2) .0403(12) C8 .5234(3) .1715(3) -.0853(2) .050(2) C9 .5574(4) .2422(3) -.1392(3) .060(2) C10 .5810(4) .3483(4) -.1142(3) .068(2) C11 .5681(4) .3831(3) -.0355(3) .064(2) C12 .5334(4) .3134(3) .0181(3) .056(2) C13 .7286(3) .0901(5) .1651(3) .089(2) C14 .7254(4) .2612(4) .2827(4) .105(2) C15 .6995(4) .0460(4) .3292(3) .075(2) C16 .2183(3) .0664(4) .0283(3) .078(2) C17 .2422(4) .2954(4) .0383(3) .077(2) C18 .1909(3) .1802(4) .1759(3) .078(2) H .454(3) .077(3) 0.028(2) .044(10) H2'a .4362 -.016350 .2447 .08 H2'b .34258 -.04176 .28789 .08 H2'c .47124 -.06063 .34416 .08 H3 .385(3) .058(3) .448(2) .048(10) H4'a .35636 .17588 .55529 .08 H4'b .30115 .28615 .51365 .08 H4'c .42969 .28173 .57459 .08 H5 .430(3) .376(3) .420(2) .043(9) H6'a .48194 .36413 .21388 .08 H6'b .52899 .42859 .30519 .08 H6'c .3985 .43011 .24956 .08 H8 .509(2) .098(3) -.105(2) .041(9) H9 .567(3) .218(3) -.195(2) .062(11) H10 .602(3) .391(3) -.157(3) .073(12) H11 .586(3) .455(3) -.014(2) .061(11) H12 .525(3) .339(3) .066(2) .051(10) H13a .71105 .1334 .11121 .08 H13b .70733 .01639 .14861 .08 H13c .8088 .09372 .19798 .08 H14a .69011 .29452 .32179 .08 H14b .72317 0.31011 .23445 .08 H14c .80306 .24415 .31689 .08 H15a .66441 .06312 .37347 .08347 H15b .78065 .0511 .35666 .08 H15c .67917 -.02623 .30729 .08 H16a .26019 .05582 -.01236 .08 H16b .14113 .08524 -.00581 .08 H16c .21925 .00082 .06143 .08 H17a .28634 .30069 -.00121 .08 H17b .25597 .35781 .07705 .08 H17c .1629 .29187 .00273 .08 H18a .21726 .2356 .22112 .08 H18b .19257 .1116 .20512 .08 H18c .11445 .19603 .13787 .08 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 P1 Ni P2 177.78(8) yes P1 Ni N 94.36(10) yes P2 Ni N 87.29(10) yes P2 Ni C1 88.50(10) yes N Ni C1 175.72(13) yes C1 Ni P1 89.87(10) yes C13 P1 C14 103.0(3) yes C13 P1 C15 99.8(2) yes C13 P1 Ni 116.32(12) yes C14 P1 C15 102.5(2) yes C14 P1 Ni 115.0(2) yes C15 P1 Ni 117.8(2) yes C16 P2 C17 103.5(2) yes C16 P2 C18 101.8(2) yes C16 P2 Ni 113.29(15) yes C17 P2 C18 102.6(2) yes C17 P2 Ni 112.2(2) yes C18 P2 Ni 121.42(12) yes C7 N Ni 129.9(2) yes C2 C1 C6 116.5(3) yes C2 C1 Ni 121.6(3) yes C6 C1 Ni 121.5(3) yes C2' C2 C3 119.2(4) yes C2' C2 C1 119.6(4) yes C3 C2 C1 121.0(3) yes C4 C3 C2 122.1(4) yes C4' C4 C5 120.9(4) yes C4' C4 C3 121.8(4) yes C5 C4 C3 117.2(4) yes C6 C5 C4 122.5(4) yes C6' C6 C1 121.2(3) yes C6' C6 C5 118.1(3) yes C1 C6 C5 120.6(3) yes C8 C7 C12 115.2(4) yes C8 C7 N 123.0(3) yes C12 C7 N 121.8(4) yes C9 C8 C7 121.8(4) yes C10 C9 C8 120.9(4) yes C11 C10 C9 118.6(5) yes C12 C11 C10 120.8(4) yes C7 C12 C11 122.6(4) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag P1 Ni 2.1900(10) yes P2 Ni 2.1820(10) yes N Ni 1.932(3) yes C1 Ni 1.910(4) yes C13 P1 1.807(5) yes C14 P1 1.789(5) yes C15 P1 1.811(4) yes C16 P2 1.819(4) yes C17 P2 1.809(4) yes C18 P2 1.819(5) yes C7 N 1.354(5) yes C2 C1 1.411(5) yes C6 C1 1.405(5) yes C2' C2 1.502(5) yes C3 C2 1.390(6) yes C4 C3 1.379(6) yes C4' C4 1.512(6) yes C5 C4 1.376(6) yes C6 C5 1.394(6) yes C6' C6 1.511(5) yes C8 C7 1.404(5) yes C12 C7 1.394(5) yes C9 C8 1.378(6) yes C10 C9 1.372(6) yes C11 C10 1.366(7) yes C12 C11 1.372(7) yes H N .82(3) no H2'a C2' .960(5) no H2'b C2' .960(4) no H2'c C2' .960(3) no H3 C3 .99(4) no H4'a C4' .960(5) no H4'b C4' .960(4) no H4'c C4' .960(4) no H5 C5 .93(3) no H6'a C6' .960(5) no H6'b C6' .960(4) no H6'c C6' .960(4) no H8 C8 .96(3) no H9 C9 .97(4) no H10 C10 .95(4) no H11 C11 .95(4) no H12 C12 .86(4) no H13a C13 .960(5) no H13b C13 .960(5) no H13c C13 .960(4) no H14a C14 .960(6) no H14b C14 .960(6) no H14c C14 .960(4) no H15a C15 .960(5) no H15b C15 .960(4) no H15c C15 .960(4) no H16a C16 .960(5) no H16b C16 .960(4) no H16c C16 .960(5) no H17a C17 .960(5) no H17b C17 .960(4) no H17c C17 .960(4) no H18a C18 .960(4) no H18b C18 .960(5) no H18c C18 .960(4) no