#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/01/2200171.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_2200171 loop_ _publ_author_name 'Twamley, Brendan' 'Zehnder, Ralph' 'Shapiro, Pamela J.' _publ_section_title ; Solvated CrBr~2~(thf)~2~, a linear chain in the solid state ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m80 _journal_page_last m81 _journal_paper_doi 10.1107/S1600536801001660 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cr Br2 (C4 H8 O)2]' _chemical_formula_moiety 'C8 H16 Br2 Cr O2' _chemical_formula_sum 'C8 H16 Br2 Cr O2' _chemical_formula_weight 356.03 _chemical_name_common CrBr2.2THF _chemical_name_systematic ; dibromobis(tetrahydrofuran-O)chromium(II) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-97 _cell_angle_alpha 87.777(3) _cell_angle_beta 78.619(3) _cell_angle_gamma 87.281(3) _cell_formula_units_Z 1 _cell_length_a 4.1043(7) _cell_length_b 7.4530(13) _cell_length_c 9.2875(16) _cell_measurement_reflns_used 839 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 2.2 _cell_volume 278.07(8) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT-Plus (Bruker, 1999)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _diffrn_ambient_temperature 203(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full .992 _diffrn_measured_fraction_theta_max .992 _diffrn_measurement_device_type 'Siemens SMART 1000' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0290 _diffrn_reflns_av_sigmaI/netI .0307 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2917 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.2 _diffrn_standards_decay_% <0.01 _diffrn_standards_interval_count 'beginning and end' _diffrn_standards_number '50 frames remeasured' _exptl_absorpt_coefficient_mu 8.18 _exptl_absorpt_correction_T_max .293 _exptl_absorpt_correction_T_min .184 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1999)' _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 174 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .15 _refine_diff_density_max .577 _refine_diff_density_min -.701 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 61 _refine_ls_number_reflns 962 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.08 _refine_ls_R_factor_all .031 _refine_ls_R_factor_gt .027 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.1523P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .071 _reflns_number_gt 897 _reflns_number_total 962 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file na6034.cif _[local]_cod_data_source_block bt172 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2200171 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Br1 .10559(9) .70378(5) .37413(4) .02022(17) Uani d . 1 . . Br Cr1 .5000 .5000 .5000 .0180(2) Uani d S 1 . . Cr O1 .4032(7) .6622(3) .6810(3) .0245(6) Uani d . 1 . . O C1 .2743(10) .5980(5) .8298(4) .0242(9) Uani d . 1 . . C H1A .3974 .4886 .8536 .029 Uiso calc R 1 . . H H1B .0382 .5724 .8425 .029 Uiso calc R 1 . . H C3 .2812(11) .9167(5) .8283(4) .0244(9) Uani d . 1 . . C H3A .0454 .9507 .8342 .029 Uiso calc R 1 . . H H3B .3948 1.0190 .8558 .029 Uiso calc R 1 . . H C2 .3237(10) .7515(5) .9266(4) .0240(9) Uani d . 1 . . C H2A .5459 .7433 .9508 .029 Uiso calc R 1 . . H H2B .1558 .7528 1.0177 .029 Uiso calc R 1 . . H C4 .4399(10) .8560(5) .6761(4) .0232(9) Uani d . 1 . . C H4A .3266 .9144 .6022 .028 Uiso calc R 1 . . H H4B .6753 .8848 .6524 .028 Uiso calc R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 .0210(2) .0198(2) .0199(3) .00074(15) -.00461(16) .00071(15) Cr1 .0230(5) .0167(4) .0144(5) .0034(3) -.0046(4) -.0026(3) O1 .0390(16) .0173(13) .0152(14) -.0007(12) -.0004(12) -.0019(11) C1 .029(2) .022(2) .018(2) .0006(16) .0015(17) -.0007(16) C3 .027(2) .024(2) .021(2) .0004(16) -.0020(17) -.0058(16) C2 .028(2) .027(2) .017(2) .0021(17) -.0026(17) -.0052(17) C4 .032(2) .0162(19) .021(2) -.0041(16) -.0036(17) -.0010(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1 Cr1 O1 2_666 . 180.00(9) O1 Cr1 Br1 2_666 2_666 90.09(8) O1 Cr1 Br1 . 2_666 89.91(8) O1 Cr1 Br1 2_666 . 89.91(8) O1 Cr1 Br1 . . 90.09(8) Br1 Cr1 Br1 2_666 . 180.0 C1 O1 C4 . . 110.7(3) C1 O1 Cr1 . . 124.1(2) C4 O1 Cr1 . . 125.1(2) O1 C1 C2 . . 104.7(3) C4 C3 C2 . . 103.6(3) C1 C2 C3 . . 102.1(3) O1 C4 C3 . . 105.2(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 Cr1 . 2.5825(5) ? Cr1 O1 2_666 2.072(3) ? Cr1 O1 . 2.072(3) ? Cr1 Br1 2_666 2.5825(5) ? O1 C1 . 1.450(5) ? O1 C4 . 1.458(4) ? C1 C2 . 1.527(6) ? C3 C4 . 1.512(5) ? C3 C2 . 1.528(6) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C4 H4A Br1 . .98 2.99 3.599(4) 121.6 C1 H1A Br1 2_666 .98 2.99 3.607(4) 121.9