#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/20/2012059.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_2012059 loop_ _publ_author_name 'Naumov, Dmitry Yu.' 'Yufit, Dmitrii S.' 'Boldyreva, Elena V.' 'Howard, Judith A. K.' _publ_section_title ; A urea complex of copper(II) hypophosphite at 293, 100 and 15K ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 790 _journal_page_last 792 _journal_paper_doi 10.1107/S0108270101004711 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu (H2 P O2)2 (C H4 N2 O)]' _chemical_formula_moiety 'C H8 Cu N2 O5 P2' _chemical_formula_sum 'C H8 Cu N2 O5 P2' _chemical_formula_weight 253.57 _chemical_name_systematic ; poly[copper(II)-di-\m-hypophosphito-\m-urea] ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 100.2722(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.5540(3) _cell_length_b 7.4686(2) _cell_length_c 8.2628(3) _cell_measurement_reflns_used 2732 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.09 _cell_measurement_theta_min 3.19 _cell_volume 762.31(4) _computing_cell_refinement 'SAINT (Siemens, 1994)' _computing_data_collection 'SMART (Siemens, 1994)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 8.192 _diffrn_measured_fraction_theta_full .991 _diffrn_measured_fraction_theta_max .991 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .030 _diffrn_reflns_av_sigmaI/netI .033 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2894 _diffrn_reflns_theta_full 29.09 _diffrn_reflns_theta_max 29.09 _diffrn_reflns_theta_min 3.19 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 3.263 _exptl_absorpt_correction_T_max .488 _exptl_absorpt_correction_T_min .221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 2.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 508 _exptl_crystal_size_max .54 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .22 _refine_diff_density_max .40 _refine_diff_density_min -.73 _refine_ls_extinction_coef .026(2) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 70 _refine_ls_number_reflns 1014 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.119 _refine_ls_R_factor_all .028 _refine_ls_R_factor_gt .026 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0471P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .076 _reflns_number_gt 920 _reflns_number_total 1014 _reflns_threshold_expression I>2\s(I) _cod_data_source_file av1072.cif _cod_data_source_block Iat293K _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times). 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 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times). '_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times). '_geom_torsion_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_hbond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times). '_geom_hbond_publ_flag' value 'No' changed to 'no' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (3 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2012059 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Cu1 0 0 0.5 .01994(17) Uani d S 1 . . Cu P1 .17206(4) -.12420(7) 0.29901(6) .02362(18) Uani d . 1 . . P H1 .259(2) -.227(4) 0.332(4) .036(7) Uiso d . 1 . . H H2 .204(2) .056(5) 0.337(4) .044(8) Uiso d . 1 . . H O1 .09677(12) -.17305(18) 0.41699(17) .0245(3) Uani d . 1 . . O O2 .12775(12) -.1344(2) 0.11669(18) .0278(3) Uani d . 1 . . O O3 0 .1676(3) 0.25 .0262(4) Uani d S 1 . . O C1 0 .3358(4) 0.25 .0248(5) Uani d S 1 . . C N1 .0690(2) .4284(3) 0.3625(3) .0390(5) Uani d . 1 . . N H3 .062(3) .529(5) 0.380(4) .033(8) Uiso d . 1 . . H H4 .099(4) .382(6) 0.437(6) .069(14) Uiso d . 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 Cu1 .0259(2) .0190(2) .0146(2) -.00243(10) .00285(13) -.00262(10) P1 .0253(3) .0269(3) .0178(3) .00247(18) .00147(18) .00155(18) O1 .0345(7) .0190(7) .0208(6) .0029(5) .0069(6) .0027(5) O2 .0328(7) .0322(8) .0180(6) .0100(6) .0032(6) .0028(5) O3 .0422(11) .0149(9) .0212(9) 0 .0051(8) 0 C1 .0351(14) .0193(12) .0231(12) 0 .0133(11) 0 N1 .0571(13) .0207(10) .0380(11) -.0077(9) .0050(10) -.0063(8) 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' N N .0061 .0033 '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' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .3201 1.2651 '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 _geom_angle_publ_flag O1 Cu1 O1 5_556 . 180.0 ? O1 Cu1 O2 5_556 2 90.34(6) ? O1 Cu1 O2 . 2 89.66(6) ? O1 Cu1 O2 5_556 6_556 89.66(6) ? O1 Cu1 O2 . 6_556 90.34(6) yes O2 Cu1 O2 2 6_556 180.00(6) ? O1 Cu1 O3 5_556 . 92.96(5) ? O1 Cu1 O3 . . 87.04(5) yes O2 Cu1 O3 2 . 88.28(5) ? O2 Cu1 O3 6_556 . 91.72(5) yes O1 Cu1 O3 5_556 5_556 87.04(5) ? O1 Cu1 O3 . 5_556 92.96(5) ? O2 Cu1 O3 2 5_556 91.72(5) ? O2 Cu1 O3 6_556 5_556 88.28(5) ? O3 Cu1 O3 . 5_556 180.0 ? O1 Cu1 Cu1 5_556 2 117.14(4) ? O1 Cu1 Cu1 . 2 62.86(4) ? O2 Cu1 Cu1 2 2 70.07(4) ? O2 Cu1 Cu1 6_556 2 109.93(4) ? O3 Cu1 Cu1 . 2 31.21(4) ? O3 Cu1 Cu1 5_556 2 148.79(4) ? O1 P1 O2 . . 117.84(8) yes O1 P1 H1 . . 108.5(13) yes O2 P1 H1 . . 108.5(14) yes O1 P1 H2 . . 105.5(13) yes O2 P1 H2 . . 107.8(14) yes H1 P1 H2 . . 108.3(17) yes P1 O1 Cu1 . . 123.82(8) yes P1 O2 Cu1 . 2 125.38(9) yes C1 O3 Cu1 . 2 121.21(4) ? C1 O3 Cu1 . . 121.21(4) yes Cu1 O3 Cu1 2 . 117.57(8) yes O3 C1 N1 . . 120.97(15) yes O3 C1 N1 . 2 120.97(15) ? N1 C1 N1 . 2 118.1(3) yes C1 N1 H3 . . 123(2) ? C1 N1 H4 . . 120(3) ? H3 N1 H4 . . 111(4) ? 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 Cu1 O1 5_556 1.9784(14) ? Cu1 O1 . 1.9784(14) yes Cu1 O2 2 1.9895(14) ? Cu1 O2 6_556 1.9895(14) yes Cu1 O3 . 2.4153(10) yes Cu1 O3 5_556 2.4153(10) ? Cu1 Cu1 2 4.13140(15) yes P1 O1 . 1.5184(15) yes P1 O2 . 1.5119(15) yes P1 H1 . 1.32(3) yes P1 H2 . 1.42(4) yes O2 Cu1 2 1.9895(14) ? O3 C1 . 1.256(3) yes O3 Cu1 2 2.4154(10) ? C1 N1 . 1.344(3) yes C1 N1 2 1.344(3) ? N1 H3 . .77(3) ? N1 H4 . .75(5) ? 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 _geom_hbond_publ_flag N1 H4 O2 6_556 .75(5) 2.36(5) 3.037(3) 152(4) yes P1 H2 O3 . 1.42(4) 2.66(3) 3.0442(14) 91.2(13) no P1 H2 O2 6_556 1.42(4) 2.72(3) 3.3840(16) 105.4(17) no N1 H3 O1 1_565 .77(3) 2.27(4) 3.021(3) 162(3) yes P1 H1 O1 7_546 1.32(3) 2.61(3) 3.7139(15) 139(2) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag N1 C1 O3 Cu1 47.74(12) yes