#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/15/7011535.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_7011535
loop_
_publ_author_name
'Kontturi, Mervi'
'Vuokila-Laine, Eija'
'Peräniemi, Sirpa'
'Pakkanen, Tuula T.'
'Vepsäläinen, Jouko J.'
'Ahlgrén, Markku'
_publ_section_title
;
 A structural study of bisphosphonate metal complexes. Alkaline earth
 metal complexes of (dichloromethylene)bisphosphonic acid P,P'-diethyl
 ester
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1969
_journal_paper_doi               10.1039/b201124g
_journal_year                    2002
_chemical_formula_moiety         '[MgCl2C(PO3Et)2(H2O)3]n'
_chemical_formula_sum            'C5 H16 Cl2 Mg O9 P2'
_chemical_formula_weight         377.33
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.151(6)
_cell_angle_beta                 97.755(5)
_cell_angle_gamma                93.418(7)
_cell_formula_units_Z            2
_cell_length_a                   7.3862(7)
_cell_length_b                   8.3578(7)
_cell_length_c                   11.8701(11)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.79
_cell_volume                     722.38(11)
_computing_cell_refinement       'Denzo, Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'collect (Nonius, 1999)'
_computing_data_reduction        'Denzo, Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       phi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11038
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.8351
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      1.704(14)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       plate
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0108(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0392
_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)+(0.0200P)²+0.8000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                2631
_reflns_number_total             3041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201124g.txt
_cod_data_source_block           Structure_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               7011535
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.26984(8) 0.20308(7) 0.85353(5) 0.02113(16) Uani 1 1 d . . .
Cl2 Cl 0.59171(8) 0.40530(8) 0.82710(5) 0.02192(16) Uani 1 1 d . . .
Mg1 Mg 0.5000 0.5000 0.5000 0.0153(2) Uani 1 2 d S . .
Mg2 Mg 0.0000 0.0000 0.5000 0.0159(2) Uani 1 2 d S . .
P1 P 0.22893(8) 0.47493(7) 0.70577(5) 0.01486(16) Uani 1 1 d . . .
P2 P 0.42423(8) 0.18011(7) 0.63137(5) 0.01438(15) Uani 1 1 d . . .
O1 O 0.2643(2) 0.4041(2) 0.38570(15) 0.0187(4) Uani 1 1 d . . .
O2 O -0.0548(2) 0.2368(2) 0.46584(14) 0.0194(4) Uani 1 1 d . . .
O3 O 0.0851(2) -0.0437(2) 0.34121(15) 0.0218(4) Uani 1 1 d . . .
O11 O 0.3232(2) 0.5530(2) 0.61815(14) 0.0170(4) Uani 1 1 d . . .
O12 O 0.0389(2) 0.3992(2) 0.67271(14) 0.0182(4) Uani 1 1 d . . .
O13 O 0.2391(2) 0.6038(2) 0.81065(15) 0.0194(4) Uani 1 1 d . . .
O21 O 0.5335(2) 0.28048(19) 0.56264(14) 0.0166(4) Uani 1 1 d . . .
O22 O 0.2461(2) 0.0984(2) 0.57656(14) 0.0182(4) Uani 1 1 d . . .
O23 O 0.5554(2) 0.0570(2) 0.68852(14) 0.0175(4) Uani 1 1 d . . .
C1 C 0.3774(3) 0.3155(3) 0.7546(2) 0.0167(5) Uani 1 1 d . . .
C13 C 0.1111(4) 0.6056(3) 0.8930(2) 0.0255(6) Uani 1 1 d . . .
H13A H 0.1493 0.5349 0.9540 0.031 Uiso 1 1 calc R . .
H13B H -0.0130 0.5663 0.8553 0.031 Uiso 1 1 calc R . .
C14 C 0.1101(4) 0.7761(4) 0.9425(3) 0.0347(7) Uani 1 1 d . . .
H14A H 0.2331 0.8131 0.9805 0.052 Uiso 1 1 calc R . .
H14B H 0.0232 0.7814 0.9979 0.052 Uiso 1 1 calc R . .
H14C H 0.0733 0.8450 0.8812 0.052 Uiso 1 1 calc R . .
C23 C 0.4896(3) -0.0975(3) 0.7266(2) 0.0203(5) Uani 1 1 d . . .
H23A H 0.5051 -0.1867 0.6699 0.024 Uiso 1 1 calc R . .
H23B H 0.3581 -0.0963 0.7346 0.024 Uiso 1 1 calc R . .
C24 C 0.5996(4) -0.1204(3) 0.8391(2) 0.0293(6) Uani 1 1 d . . .
H24A H 0.7300 -0.1169 0.8310 0.044 Uiso 1 1 calc R . .
H24B H 0.5621 -0.2248 0.8645 0.044 Uiso 1 1 calc R . .
H24C H 0.5785 -0.0345 0.8956 0.044 Uiso 1 1 calc R . .
H1A H 0.1912 0.4748 0.3608 0.030 Uiso 1 1 d . . .
H1B H 0.1787 0.3303 0.4043 0.030 Uiso 1 1 d . . .
H2A H -0.0283 0.2967 0.5297 0.030 Uiso 1 1 d . . .
H2B H -0.1624 0.2739 0.4351 0.030 Uiso 1 1 d . . .
H3A H 0.1983 -0.0529 0.3404 0.030 Uiso 1 1 d . . .
H3B H 0.0250 -0.1326 0.3094 0.030 Uiso 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'
Mg Mg 0.0486 0.0363 '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'
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
_geom_angle_publ_flag
O21 Mg1 O21 180.0 . 2_666 ?
O21 Mg1 O11 90.06(6) . 2_666 ?
O21 Mg1 O11 89.94(6) 2_666 2_666 ?
O21 Mg1 O11 89.94(6) . . ?
O21 Mg1 O11 90.06(6) 2_666 . ?
O11 Mg1 O11 180.000(1) 2_666 . ?
O21 Mg1 O1 89.16(7) . 2_666 ?
O21 Mg1 O1 90.84(7) 2_666 2_666 ?
O11 Mg1 O1 87.24(7) 2_666 2_666 ?
O11 Mg1 O1 92.76(7) . 2_666 ?
O21 Mg1 O1 90.84(7) . . ?
O21 Mg1 O1 89.16(7) 2_666 . ?
O11 Mg1 O1 92.76(7) 2_666 . ?
O11 Mg1 O1 87.24(7) . . ?
O1 Mg1 O1 180.0 2_666 . ?
O22 Mg2 O22 180.0 2_556 . ?
O22 Mg2 O3 85.35(7) 2_556 . ?
O22 Mg2 O3 94.65(7) . . ?
O22 Mg2 O3 94.65(7) 2_556 2_556 ?
O22 Mg2 O3 85.35(7) . 2_556 ?
O3 Mg2 O3 180.0 . 2_556 ?
O22 Mg2 O2 84.96(7) 2_556 2_556 ?
O22 Mg2 O2 95.04(7) . 2_556 ?
O3 Mg2 O2 88.61(7) . 2_556 ?
O3 Mg2 O2 91.39(7) 2_556 2_556 ?
O22 Mg2 O2 95.04(7) 2_556 . ?
O22 Mg2 O2 84.96(7) . . ?
O3 Mg2 O2 91.39(7) . . ?
O3 Mg2 O2 88.61(7) 2_556 . ?
O2 Mg2 O2 180.0 2_556 . ?
O11 P1 O12 119.23(10) . . ?
O11 P1 O13 106.56(10) . . ?
O12 P1 O13 111.28(10) . . ?
O11 P1 C1 105.16(10) . . ?
O12 P1 C1 107.61(10) . . ?
O13 P1 C1 106.13(10) . . ?
O21 P2 O22 119.15(10) . . ?
O21 P2 O23 107.38(9) . . ?
O22 P2 O23 111.53(10) . . ?
O21 P2 C1 106.30(10) . . ?
O22 P2 C1 107.58(10) . . ?
O23 P2 C1 103.72(10) . . ?
Mg1 O1 H1A 115 . . ?
Mg1 O1 H1B 124 . . ?
H1A O1 H1B 99 . . ?
Mg2 O2 H2A 108 . . ?
Mg2 O2 H2B 128 . . ?
H2A O2 H2B 102 . . ?
Mg2 O3 H3A 117 . . ?
Mg2 O3 H3B 107 . . ?
H3A O3 H3B 109 . . ?
P1 O11 Mg1 140.29(10) . . ?
C13 O13 P1 124.48(16) . . ?
P2 O21 Mg1 133.02(10) . . ?
P2 O22 Mg2 176.77(11) . . ?
C23 O23 P2 123.64(15) . . ?
Cl2 C1 Cl1 107.98(12) . . ?
Cl2 C1 P1 109.58(13) . . ?
Cl1 C1 P1 109.35(12) . . ?
Cl2 C1 P2 108.27(12) . . ?
Cl1 C1 P2 110.63(13) . . ?
P1 C1 P2 110.98(12) . . ?
O13 C13 C14 107.6(2) . . ?
O13 C13 H13A 110.2 . . ?
C14 C13 H13A 110.2 . . ?
O13 C13 H13B 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O23 C23 C24 108.0(2) . . ?
O23 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
O23 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1 1.793(2) . ?
Cl2 C1 1.791(2) . ?
Mg1 O21 2.0451(16) . ?
Mg1 O21 2.0451(16) 2_666 ?
Mg1 O11 2.0834(16) 2_666 ?
Mg1 O11 2.0834(16) . ?
Mg1 O1 2.1338(17) 2_666 ?
Mg1 O1 2.1338(17) . ?
Mg2 O22 2.0187(16) 2_556 ?
Mg2 O22 2.0187(16) . ?
Mg2 O3 2.0806(18) . ?
Mg2 O3 2.0806(17) 2_556 ?
Mg2 O2 2.1006(17) 2_556 ?
Mg2 O2 2.1006(17) . ?
P1 O11 1.4941(17) . ?
P1 O12 1.4945(17) . ?
P1 O13 1.5769(18) . ?
P1 C1 1.852(2) . ?
P2 O21 1.4889(17) . ?
P2 O22 1.4891(17) . ?
P2 O23 1.5812(17) . ?
P2 C1 1.866(3) . ?
O1 H1A 0.87 . ?
O1 H1B 0.92 . ?
O2 H2A 0.87 . ?
O2 H2B 0.91 . ?
O3 H3A 0.85 . ?
O3 H3B 0.88 . ?
O13 C13 1.449(3) . ?
O23 C23 1.475(3) . ?
C13 C14 1.502(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C23 C24 1.498(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1B O2 0.92 2.09 2.969(2) 160 .
O1 H1A O12 0.87 2.06 2.895(2) 162 2_566
O2 H2A O12 0.87 1.84 2.702(2) 172 .
O2 H2B O11 0.91 2.01 2.854(2) 154 2_566
O3 H3A O23 0.85 1.90 2.733(2) 169 2_656
O3 H3B O12 0.88 2.28 3.043(3) 145 2_556
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12 P1 O11 Mg1 -93.07(17) . . . . ?
O13 P1 O11 Mg1 140.03(15) . . . . ?
C1 P1 O11 Mg1 27.64(19) . . . . ?
O21 Mg1 O11 P1 -7.02(17) . . . . ?
O21 Mg1 O11 P1 172.98(17) 2_666 . . . ?
O11 Mg1 O11 P1 -167(100) 2_666 . . . ?
O1 Mg1 O11 P1 -96.17(17) 2_666 . . . ?
O1 Mg1 O11 P1 83.83(17) . . . . ?
O11 P1 O13 C13 155.00(19) . . . . ?
O12 P1 O13 C13 23.5(2) . . . . ?
C1 P1 O13 C13 -93.3(2) . . . . ?
O22 P2 O21 Mg1 72.06(16) . . . . ?
O23 P2 O21 Mg1 -160.00(12) . . . . ?
C1 P2 O21 Mg1 -49.49(16) . . . . ?
O21 Mg1 O21 P2 37(100) 2_666 . . . ?
O11 Mg1 O21 P2 -160.33(14) 2_666 . . . ?
O11 Mg1 O21 P2 19.67(14) . . . . ?
O1 Mg1 O21 P2 112.43(14) 2_666 . . . ?
O1 Mg1 O21 P2 -67.57(14) . . . . ?
O21 P2 O22 Mg2 -57(2) . . . . ?
O23 P2 O22 Mg2 177(100) . . . . ?
C1 P2 O22 Mg2 64(2) . . . . ?
O22 Mg2 O22 P2 -34(100) 2_556 . . . ?
O3 Mg2 O22 P2 92(2) . . . . ?
O3 Mg2 O22 P2 -88(2) 2_556 . . . ?
O2 Mg2 O22 P2 -179(100) 2_556 . . . ?
O2 Mg2 O22 P2 1(2) . . . . ?
O21 P2 O23 C23 -156.50(17) . . . . ?
O22 P2 O23 C23 -24.3(2) . . . . ?
C1 P2 O23 C23 91.23(19) . . . . ?
O11 P1 C1 Cl2 65.84(14) . . . . ?
O12 P1 C1 Cl2 -166.07(11) . . . . ?
O13 P1 C1 Cl2 -46.85(14) . . . . ?
O11 P1 C1 Cl1 -175.99(11) . . . . ?
O12 P1 C1 Cl1 -47.90(15) . . . . ?
O13 P1 C1 Cl1 71.32(14) . . . . ?
O11 P1 C1 P2 -53.67(14) . . . . ?
O12 P1 C1 P2 74.41(14) . . . . ?
O13 P1 C1 P2 -166.36(11) . . . . ?
O21 P2 C1 Cl2 -54.91(14) . . . . ?
O22 P2 C1 Cl2 176.41(11) . . . . ?
O23 P2 C1 Cl2 58.14(14) . . . . ?
O21 P2 C1 Cl1 -173.05(11) . . . . ?
O22 P2 C1 Cl1 58.27(14) . . . . ?
O23 P2 C1 Cl1 -59.99(14) . . . . ?
O21 P2 C1 P1 65.38(14) . . . . ?
O22 P2 C1 P1 -63.29(14) . . . . ?
O23 P2 C1 P1 178.44(11) . . . . ?
P1 O13 C13 C14 -154.18(19) . . . . ?
P2 O23 C23 C24 -138.54(19) . . . . ?
