#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:49:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324617.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_4324617
loop_
_publ_author_name
'Deng-Ke Cao'
'Mei-Juan Liu'
'Jian Huang'
'Song-Song Bao'
'Li-Min Zheng'
_publ_section_title
;
 Cobalt and Manganese Diphosphonates with One-, Two-, and
 Three-Dimensional Structures and Field-Induced Magnetic Transitions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2278
_journal_page_last               2287
_journal_paper_doi               10.1021/ic1019668
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C10 H22 Co3 N4 O18 P4'
_chemical_formula_sum            'C10 H22 Co3 N4 O18 P4'
_chemical_formula_weight         786.99
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.14
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.496(3)
_cell_length_b                   9.469(2)
_cell_length_c                   19.485(4)
_cell_measurement_reflns_used    1399
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.315
_cell_measurement_theta_min      2.706
_cell_volume                     2305.5(9)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6790
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    2.509
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0363
_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)+(0.0550P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                1649
_reflns_number_total             2084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1019668_si_004.cif
_cod_data_source_block           co
_cod_original_cell_volume        2305.5(8)
_cod_database_code               4324617
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_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
Co1 Co 0.24003(5) 0.37210(6) 0.34048(3) 0.0162(2) Uani 1 1 d .
Co2 Co 0.0000 0.56674(9) 0.2500 0.0152(2) Uani 1 2 d S
P1 P 0.26643(9) 0.56997(11) 0.23849(5) 0.0121(3) Uani 1 1 d .
P2 P 0.14047(9) 0.59418(11) 0.10493(5) 0.0136(3) Uani 1 1 d .
O1 O 0.1608(2) 0.5510(3) 0.27594(14) 0.0182(7) Uani 1 1 d .
O1W O 0.1200(3) 0.4026(3) 0.40390(16) 0.0274(8) Uani 1 1 d .
H1WA H 0.1308 0.4062 0.4471 0.033 Uiso 1 1 d R
H1WB H 0.0557 0.3970 0.3895 0.033 Uiso 1 1 d R
O2 O 0.3463(2) 0.4804(3) 0.27910(15) 0.0181(7) Uani 1 1 d .
O2W O 0.0000 0.3421(5) 0.2500 0.0350(13) Uani 1 2 d S
H2WA H -0.0541 0.3055 0.2302 0.042 Uiso 0.50 1 d PR
H2WB H 0.0539 0.3180 0.2259 0.042 Uiso 0.50 1 d PR
O3 O 0.3039(2) 0.7222(3) 0.23003(14) 0.0147(7) Uani 1 1 d .
O3W O 0.0000 0.7862(5) 0.2500 0.0416(14) Uani 1 2 d S
H3WA H 0.0391 0.8094 0.2159 0.050 Uiso 0.50 1 d PR
H3WB H -0.0607 0.8237 0.2418 0.050 Uiso 0.50 1 d PR
O4 O 0.0401(2) 0.5647(3) 0.14669(14) 0.0185(7) Uani 1 1 d .
O5 O 0.1699(2) 0.7504(3) 0.10262(15) 0.0198(7) Uani 1 1 d .
O6 O 0.1332(2) 0.5289(3) 0.03390(14) 0.0196(7) Uani 1 1 d .
O7 O 0.2257(3) 0.3552(3) 0.14875(15) 0.0217(7) Uani 1 1 d .
H7A H 0.2184 0.3263 0.1881 0.032 Uiso 1 1 calc R
N1 N 0.3747(3) 0.4331(4) 0.05417(19) 0.0177(8) Uani 1 1 d .
N2 N 0.3893(3) 0.2487(4) -0.0107(2) 0.0283(10) Uani 1 1 d .
H2A H 0.3962 0.1624 -0.0239 0.034 Uiso 1 1 calc R
C1 C 0.2526(3) 0.5020(4) 0.1501(2) 0.0151(10) Uani 1 1 d .
C2 C 0.3630(4) 0.5189(5) 0.1155(2) 0.0193(10) Uani 1 1 d .
H2B H 0.3733 0.6174 0.1034 0.023 Uiso 1 1 calc R
H2C H 0.4184 0.4932 0.1481 0.023 Uiso 1 1 calc R
C3 C 0.3864(4) 0.2922(5) 0.0534(2) 0.0255(11) Uani 1 1 d .
H3B H 0.3917 0.2346 0.0919 0.031 Uiso 1 1 calc R
C4 C 0.3796(4) 0.3636(5) -0.0530(2) 0.0293(12) Uani 1 1 d .
H4A H 0.3796 0.3624 -0.1007 0.035 Uiso 1 1 calc R
C5 C 0.3700(4) 0.4788(5) -0.0127(2) 0.0236(11) Uani 1 1 d .
H5B H 0.3619 0.5716 -0.0274 0.028 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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
O5 Co1 O1W 99.75(13) 4_545 .
O5 Co1 O3 97.17(12) 4_545 4_545
O1W Co1 O3 108.62(13) . 4_545
O5 Co1 O2 104.55(13) 4_545 .
O1W Co1 O2 141.67(13) . .
O3 Co1 O2 97.33(12) 4_545 .
O5 Co1 O1 168.18(11) 4_545 .
O1W Co1 O1 84.75(12) . .
O3 Co1 O1 91.65(10) 4_545 .
O2 Co1 O1 66.36(11) . .
O3W Co2 O1 94.12(8) . 2
O3W Co2 O1 94.12(8) . .
O1 Co2 O1 171.76(17) 2 .
O3W Co2 O4 90.54(9) . .
O1 Co2 O4 89.93(11) 2 .
O1 Co2 O4 90.00(11) . .
O3W Co2 O4 90.54(9) . 2
O1 Co2 O4 90.00(11) 2 2
O1 Co2 O4 89.93(11) . 2
O4 Co2 O4 178.92(17) . 2
O3W Co2 O2W 180.000(1) . .
O1 Co2 O2W 85.88(8) 2 .
O1 Co2 O2W 85.88(8) . .
O4 Co2 O2W 89.46(9) . .
O4 Co2 O2W 89.46(9) 2 .
O1 P1 O3 115.53(17) . .
O1 P1 O2 104.65(17) . .
O3 P1 O2 112.32(16) . .
O1 P1 C1 109.06(18) . .
O3 P1 C1 104.90(17) . .
O2 P1 C1 110.42(18) . .
O6 P2 O4 111.38(17) . .
O6 P2 O5 112.45(17) . .
O4 P2 O5 113.12(18) . .
O6 P2 C1 106.43(18) . .
O4 P2 C1 106.25(18) . .
O5 P2 C1 106.66(17) . .
P1 O1 Co2 135.70(17) . .
P1 O1 Co1 88.64(14) . .
Co2 O1 Co1 126.43(14) . .
Co1 O1W H1WA 120.4 . .
Co1 O1W H1WB 120.2 . .
H1WA O1W H1WB 118.3 . .
P1 O2 Co1 98.92(16) . .
Co2 O2W H2WA 114.0 . .
Co2 O2W H2WB 105.5 . .
H2WA O2W H2WB 105.5 . .
P1 O3 Co1 130.19(16) . 4
Co2 O3W H3WA 104.9 . .
Co2 O3W H3WB 114.6 . .
H3WA O3W H3WB 105.0 . .
P2 O4 Co2 135.84(17) . .
P2 O5 Co1 133.94(17) . 4
C1 O7 H7A 109.5 . .
C3 N1 C5 107.9(4) . .
C3 N1 C2 125.2(4) . .
C5 N1 C2 126.8(4) . .
C3 N2 C4 108.6(4) . .
C3 N2 H2A 125.7 . .
C4 N2 H2A 125.7 . .
O7 C1 C2 107.6(3) . .
O7 C1 P1 112.2(3) . .
C2 C1 P1 106.8(3) . .
O7 C1 P2 105.6(3) . .
C2 C1 P2 114.5(3) . .
P1 C1 P2 110.2(2) . .
N1 C2 C1 113.1(4) . .
N1 C2 H2B 109.0 . .
C1 C2 H2B 109.0 . .
N1 C2 H2C 109.0 . .
C1 C2 H2C 109.0 . .
H2B C2 H2C 107.8 . .
N2 C3 N1 109.0(4) . .
N2 C3 H3B 125.5 . .
N1 C3 H3B 125.5 . .
C5 C4 N2 107.5(4) . .
C5 C4 H4A 126.3 . .
N2 C4 H4A 126.3 . .
C4 C5 N1 107.0(4) . .
C4 C5 H5B 126.5 . .
N1 C5 H5B 126.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O5 1.954(3) 4_545
Co1 O1W 1.967(4) .
Co1 O3 2.050(3) 4_545
Co1 O2 2.063(3) .
Co1 O1 2.329(3) .
Co2 O3W 2.078(5) .
Co2 O1 2.076(3) 2
Co2 O1 2.076(3) .
Co2 O4 2.075(3) .
Co2 O4 2.075(3) 2
Co2 O2W 2.127(4) .
P1 O1 1.521(3) .
P1 O3 1.524(3) .
P1 O2 1.529(3) .
P1 C1 1.846(4) .
P2 O6 1.518(3) .
P2 O4 1.523(3) .
P2 O5 1.525(3) .
P2 C1 1.869(4) .
O1W H1WA 0.8530 .
O1W H1WB 0.8521 .
O2W H2WA 0.8519 .
O2W H2WB 0.8536 .
O3 Co1 2.050(3) 4
O3W H3WA 0.8539 .
O3W H3WB 0.8521 .
O5 Co1 1.954(3) 4
O7 C1 1.430(5) .
O7 H7A 0.8200 .
N1 C3 1.343(6) .
N1 C5 1.374(6) .
N1 C2 1.452(5) .
N2 C3 1.316(6) .
N2 C4 1.370(6) .
N2 H2A 0.8600 .
C1 C2 1.546(6) .
C2 H2B 0.9700 .
C2 H2C 0.9700 .
C3 H3B 0.9300 .
C4 C5 1.350(6) .
C4 H4A 0.9300 .
C5 H5B 0.9300 .
