#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/03/4330391.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_4330391
loop_
_publ_author_name
'Alexander V. Anyushin'
'Dmitry A. Mainichev'
'Nikolay K. Moroz'
'Pavel A. Abramov'
'Dmitry Yu. Naumov'
'Maxim N. Sokolov'
'Vladimir P. Fedin'
_publ_section_title
;
 Cd2+ Complexation with P(CH2OH)3, OP(CH2OH)3, and (HOCH2)2PO2-:
 Coordination in Solution and Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9995
_journal_page_last               10003
_journal_paper_doi               10.1021/ic3014283
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C3 H9 Cd1.5 Cl3 O4 P'
_chemical_formula_weight         415.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.2260(10)
_cell_angle_beta                 87.0360(10)
_cell_angle_gamma                67.1360(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9101(3)
_cell_length_b                   8.7737(3)
_cell_length_c                   9.5432(4)
_cell_measurement_temperature    150(2)
_cell_volume                     506.19(4)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker-AXS, 2004)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7088
_diffrn_reflns_theta_full        32.62
_diffrn_reflns_theta_max         32.62
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.103
_exptl_absorpt_correction_T_max  0.6844
_exptl_absorpt_correction_T_min  0.5597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.723
_exptl_crystal_description       block
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         3647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0176P)²+0.4469P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0401
_refine_ls_wR_factor_ref         0.0414
_reflns_number_gt                3336
_reflns_number_total             3647
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic3014283_si_001_1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C3 H9 Cd1.50 Cl3 O4 P'
_cod_database_code               4330391
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Cd1 Cd 1.0000 0.5000 0.0000 0.01084(4) Uani 1 2 d S
Cd2 Cd 1.029156(17) 0.096803(14) 0.294735(12) 0.01099(3) Uani 1 1 d .
P1 P 1.71402(6) -0.24855(5) 0.22941(4) 0.00916(7) Uani 1 1 d .
C2 C 1.6144(3) -0.4055(2) 0.34433(19) 0.0145(3) Uani 1 1 d .
H2A H 1.7270 -0.5237 0.3685 0.017 Uiso 1 1 calc R
H2B H 1.5738 -0.3793 0.4380 0.017 Uiso 1 1 calc R
C3 C 1.5260(2) -0.0297(2) 0.21331(18) 0.0122(3) Uani 1 1 d .
H3A H 1.5115 -0.0130 0.3119 0.015 Uiso 1 1 calc R
H3B H 1.5784 0.0560 0.1489 0.015 Uiso 1 1 calc R
C1 C 1.9401(3) -0.2666(2) 0.33323(19) 0.0137(3) Uani 1 1 d .
H1A H 1.8961 -0.2378 0.4255 0.016 Uiso 1 1 calc R
H1B H 2.0479 -0.3870 0.3595 0.016 Uiso 1 1 calc R
O1 O 2.02526(19) -0.14760(17) 0.24253(15) 0.0158(2) Uani 1 1 d .
O3 O 1.32457(18) -0.00064(15) 0.15265(13) 0.0124(2) Uani 1 1 d .
O1X O 1.76104(18) -0.27440(15) 0.07943(13) 0.0121(2) Uani 1 1 d .
O2 O 1.4363(2) -0.40121(18) 0.27123(16) 0.0193(3) Uani 1 1 d .
Cl1 Cl 0.73114(6) 0.12018(5) 0.46806(4) 0.01400(7) Uani 1 1 d .
Cl2 Cl 1.17098(6) 0.33522(5) 0.27004(4) 0.01315(7) Uani 1 1 d .
Cl3 Cl 1.22940(6) 0.68324(5) -0.07191(5) 0.01715(8) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1X Cd1 O1X 180.00(5) 1_465 2_855
O1X Cd1 Cl3 92.93(3) 1_465 2_765
O1X Cd1 Cl3 87.07(3) 2_855 2_765
O1X Cd1 Cl3 87.07(3) 1_465 .
O1X Cd1 Cl3 92.92(3) 2_855 .
Cl3 Cd1 Cl3 180.0 2_765 .
O1X Cd1 Cl2 89.76(3) 1_465 .
O1X Cd1 Cl2 90.24(3) 2_855 .
Cl3 Cd1 Cl2 84.639(13) 2_765 .
Cl3 Cd1 Cl2 95.361(13) . .
O1X Cd1 Cl2 90.24(3) 1_465 2_765
O1X Cd1 Cl2 89.76(3) 2_855 2_765
Cl3 Cd1 Cl2 95.362(13) 2_765 2_765
Cl3 Cd1 Cl2 84.639(13) . 2_765
Cl2 Cd1 Cl2 180.0 . 2_765
O1 Cd2 O3 72.25(4) 1_455 .
O1 Cd2 Cl1 95.32(3) 1_455 .
O3 Cd2 Cl1 165.75(3) . .
O1 Cd2 Cl3 93.92(3) 1_455 2_765
O3 Cd2 Cl3 95.85(3) . 2_765
Cl1 Cd2 Cl3 91.858(14) . 2_765
O1 Cd2 Cl2 153.14(3) 1_455 .
O3 Cd2 Cl2 81.05(3) . .
Cl1 Cd2 Cl2 111.541(14) . .
Cl3 Cd2 Cl2 85.802(13) 2_765 .
O1 Cd2 Cl1 87.09(3) 1_455 2_756
O3 Cd2 Cl1 88.18(3) . 2_756
Cl1 Cd2 Cl1 84.158(13) . 2_756
Cl3 Cd2 Cl1 175.968(14) 2_765 2_756
Cl2 Cd2 Cl1 95.064(13) . 2_756
O1X P1 C3 111.64(7) . .
O1X P1 C2 111.24(8) . .
C3 P1 C2 109.40(8) . .
O1X P1 C1 114.16(7) . .
C3 P1 C1 102.77(8) . .
C2 P1 C1 107.20(8) . .
O2 C2 P1 111.20(11) . .
O2 C2 H2A 109.4 . .
P1 C2 H2A 109.4 . .
O2 C2 H2B 109.4 . .
P1 C2 H2B 109.4 . .
H2A C2 H2B 108.0 . .
O3 C3 P1 110.65(11) . .
O3 C3 H3A 109.5 . .
P1 C3 H3A 109.5 . .
O3 C3 H3B 109.5 . .
P1 C3 H3B 109.5 . .
H3A C3 H3B 108.1 . .
O1 C1 P1 108.09(11) . .
O1 C1 H1A 110.1 . .
P1 C1 H1A 110.1 . .
O1 C1 H1B 110.1 . .
P1 C1 H1B 110.1 . .
H1A C1 H1B 108.4 . .
C1 O1 Cd2 124.86(10) . 1_655
C3 O3 Cd2 116.26(9) . .
P1 O1X Cd1 133.89(7) . 1_645
Cd2 Cl1 Cd2 95.843(13) . 2_756
Cd2 Cl2 Cd1 91.683(13) . .
Cd2 Cl3 Cd1 92.082(13) 2_765 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O1X 2.3379(11) 1_465
Cd1 O1X 2.3379(11) 2_855
Cd1 Cl3 2.6005(4) 2_765
Cd1 Cl3 2.6005(4) .
Cd1 Cl2 2.6154(4) .
Cd1 Cl2 2.6154(4) 2_765
Cd2 O1 2.3549(13) 1_455
Cd2 O3 2.4088(12) .
Cd2 Cl1 2.5584(4) .
Cd2 Cl3 2.5781(4) 2_765
Cd2 Cl2 2.5806(4) .
Cd2 Cl1 2.6074(4) 2_756
P1 O1X 1.5160(12) .
P1 C3 1.8166(16) .
P1 C2 1.8194(17) .
P1 C1 1.8217(17) .
C2 O2 1.428(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 O3 1.4336(19) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C1 O1 1.435(2) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
O1 Cd2 2.3549(13) 1_655
O1X Cd1 2.3379(11) 1_645
Cl1 Cd2 2.6074(4) 2_756
Cl3 Cd2 2.5780(4) 2_765
