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#$Date: 2016-03-23 16:58:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329922.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_4329922
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Joydeb Goura'
'E. Carolina Sañudo'
_publ_contact_author_address
; Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur 208016
Uttarpradesh
India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91-512-259 7436'
_publ_contact_author_name        'Prof. V. Chandrasekhar'
_publ_contact_author_phone       '+91-512-259 7259'
_publ_section_title
;
 Carboxylate-Free Manganese(II) Phosphonate Assemblies: Synthesis,
 Structure, and Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8479
_journal_page_last               8487
_journal_paper_doi               10.1021/ic301060j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C46 H70 Mn2 N6 O14 P4'
_chemical_formula_sum            'C46 H70 Mn2 N6 O14 P4'
_chemical_formula_weight         1164.87
_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                119.457(4)
_cell_angle_beta                 99.910(5)
_cell_angle_gamma                105.641(5)
_cell_formula_units_Z            1
_cell_length_a                   11.710(3)
_cell_length_b                   12.262(4)
_cell_length_c                   12.390(4)
_cell_measurement_reflns_used    3013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.19
_cell_volume                     1389.7(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  '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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7419
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.678231
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          .09
_exptl_crystal_size_mid          .07
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0496
_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)+(0.1055P)²+0.2388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                4307
_reflns_number_total             5057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301060j_si_002_1.cif
_cod_data_source_block           complex_1
_cod_database_code               4329922
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
Mn1 Mn 0.30158(4) 0.52820(4) 0.93118(4) 0.01504(18) Uani 1 1 d .
P1 P 0.42225(7) 0.29474(8) 0.82205(7) 0.0149(2) Uani 1 1 d .
P2 P 0.41716(7) 0.78431(8) 0.88733(8) 0.0167(2) Uani 1 1 d .
O4 O 0.5332(2) 0.8763(2) 1.0148(2) 0.0198(5) Uani 1 1 d .
O1 O 0.3761(2) 0.3987(2) 0.8254(2) 0.0200(5) Uani 1 1 d .
O6 O 0.3270(2) 0.6599(2) 0.8710(2) 0.0200(5) Uani 1 1 d .
O5 O 0.3381(2) 0.8668(3) 0.8781(2) 0.0219(5) Uani 1 1 d .
O3 O 0.56480(19) 0.3421(2) 0.8746(2) 0.0191(5) Uani 1 1 d .
O2 O 0.3591(2) 0.2425(2) 0.9001(2) 0.0194(5) Uani 1 1 d .
N2 N 0.1743(2) 0.4220(3) 1.0011(3) 0.0171(6) Uani 1 1 d .
O7 O 0.9286(3) 0.6625(3) 0.6011(3) 0.0395(7) Uani 1 1 d .
N1 N 0.0964(2) 0.4304(3) 0.7895(3) 0.0173(6) Uani 1 1 d .
N3 N 1.0013(3) 0.8921(3) 0.7597(3) 0.0264(7) Uani 1 1 d .
C13 C 0.3587(3) 0.1481(3) 0.6492(3) 0.0199(7) Uani 1 1 d .
C9 C 0.0467(3) 0.3606(3) 0.9308(3) 0.0168(6) Uani 1 1 d .
C1 C 0.0586(3) 0.4388(3) 0.6862(3) 0.0211(7) Uani 1 1 d .
H1 H 0.1205 0.4816 0.6650 0.025 Uiso 1 1 calc R
C4 C -0.1261(3) 0.3088(3) 0.7446(3) 0.0198(7) Uani 1 1 d .
C7 C -0.1771(3) 0.2399(3) 0.8894(3) 0.0236(7) Uani 1 1 d .
H7 H -0.2372 0.1987 0.9133 0.028 Uiso 1 1 calc R
C6 C -0.2161(3) 0.2452(3) 0.7838(3) 0.0231(7) Uani 1 1 d .
H6 H -0.3027 0.2070 0.7356 0.028 Uiso 1 1 calc R
C8 C -0.0436(3) 0.2972(3) 0.9659(3) 0.0209(7) Uani 1 1 d .
C10 C 0.0025(3) 0.2977(3) 1.0793(3) 0.0233(7) Uani 1 1 d .
H10 H -0.0541 0.2571 1.1066 0.028 Uiso 1 1 calc R
C3 C -0.1616(3) 0.3204(3) 0.6390(3) 0.0217(7) Uani 1 1 d .
H3 H -0.2473 0.2841 0.5886 0.026 Uiso 1 1 calc R
C5 C 0.0048(3) 0.3661(3) 0.8179(3) 0.0172(6) Uani 1 1 d .
C11 C 0.1305(3) 0.3581(3) 1.1489(3) 0.0255(7) Uani 1 1 d .
H11 H 0.1618 0.3582 1.2233 0.031 Uiso 1 1 calc R
C12 C 0.2150(3) 0.4204(3) 1.1067(3) 0.0216(7) Uani 1 1 d .
H12 H 0.3020 0.4616 1.1546 0.026 Uiso 1 1 calc R
C2 C -0.0693(3) 0.3861(3) 0.6088(3) 0.0246(7) Uani 1 1 d .
H2 H -0.0920 0.3950 0.5387 0.030 Uiso 1 1 calc R
C18 C 0.5631(3) 0.8616(4) 0.7662(4) 0.0320(9) Uani 1 1 d .
H18A H 0.6348 0.9119 0.8477 0.048 Uiso 1 1 calc R
H18B H 0.5195 0.9186 0.7695 0.048 Uiso 1 1 calc R
H18C H 0.5920 0.8353 0.6928 0.048 Uiso 1 1 calc R
C16 C 0.2129(3) 0.0953(4) 0.5934(4) 0.0323(8) Uani 1 1 d .
H16A H 0.1910 0.1675 0.5991 0.048 Uiso 1 1 calc R
H16B H 0.1769 0.0671 0.6443 0.048 Uiso 1 1 calc R
H16C H 0.1798 0.0184 0.5022 0.048 Uiso 1 1 calc R
C15 C 0.3940(3) 0.0325(3) 0.6417(4) 0.0283(8) Uani 1 1 d .
H15A H 0.3640 -0.0435 0.5504 0.042 Uiso 1 1 calc R
H15B H 0.3552 0.0026 0.6901 0.042 Uiso 1 1 calc R
H15C H 0.4848 0.0666 0.6799 0.042 Uiso 1 1 calc R
C20 C 0.5427(4) 0.6436(4) 0.7481(4) 0.0307(8) Uani 1 1 d .
H20A H 0.4874 0.5652 0.7417 0.046 Uiso 1 1 calc R
H20B H 0.6155 0.6975 0.8292 0.046 Uiso 1 1 calc R
H20C H 0.5701 0.6132 0.6737 0.046 Uiso 1 1 calc R
C14 C 0.4168(4) 0.1936(4) 0.5683(3) 0.0278(8) Uani 1 1 d .
H14A H 0.3852 0.1164 0.4773 0.042 Uiso 1 1 calc R
H14B H 0.5078 0.2281 0.6044 0.042 Uiso 1 1 calc R
H14C H 0.3936 0.2646 0.5725 0.042 Uiso 1 1 calc R
C19 C 0.3570(4) 0.6484(5) 0.6166(4) 0.0403(10) Uani 1 1 d .
H19A H 0.3868 0.6255 0.5441 0.060 Uiso 1 1 calc R
H19B H 0.3100 0.7024 0.6198 0.060 Uiso 1 1 calc R
H19C H 0.3027 0.5655 0.6039 0.060 Uiso 1 1 calc R
C17 C 0.4711(3) 0.7312(4) 0.7479(3) 0.0229(7) Uani 1 1 d .
C23 C 1.1074(4) 1.0186(4) 0.8658(4) 0.0402(10) Uani 1 1 d .
H23A H 1.1842 1.0041 0.8715 0.060 Uiso 1 1 calc R
H23B H 1.0942 1.0483 0.9483 0.060 Uiso 1 1 calc R
H23C H 1.1147 1.0878 0.8483 0.060 Uiso 1 1 calc R
C22 C 0.8767(4) 0.8948(5) 0.7362(4) 0.0451(11) Uani 1 1 d .
H22A H 0.8149 0.8066 0.6602 0.068 Uiso 1 1 calc R
H22B H 0.8785 0.9640 0.7200 0.068 Uiso 1 1 calc R
H22C H 0.8542 0.9155 0.8129 0.068 Uiso 1 1 calc R
C21 C 1.0145(4) 0.7756(4) 0.6876(4) 0.0312(8) Uani 1 1 d .
H21 H 1.0970 0.7806 0.7046 0.037 Uiso 1 1 calc R
H51 H 0.395(5) 0.210(5) 0.929(5) 0.066(17) Uiso 1 1 d .
H50 H 0.376(4) 0.935(4) 0.904(4) 0.018(11) 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'
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'
Mn Mn 0.3368 0.7283 '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
O1 Mn1 O6 103.05(9) . .
O1 Mn1 O3 105.40(9) . 2_667
O6 Mn1 O3 100.96(9) . 2_667
O1 Mn1 N2 106.79(9) . .
O6 Mn1 N2 144.92(9) . .
O3 Mn1 N2 88.58(9) 2_667 .
O1 Mn1 N1 103.28(9) . .
O6 Mn1 N1 83.46(9) . .
O3 Mn1 N1 149.08(9) 2_667 .
N2 Mn1 N1 72.17(10) . .
O1 P1 O3 116.11(13) . .
O1 P1 O2 107.58(13) . .
O3 P1 O2 110.59(13) . .
O1 P1 C13 107.05(14) . .
O3 P1 C13 108.41(13) . .
O2 P1 C13 106.66(14) . .
O6 P2 O4 115.18(13) . .
O6 P2 O5 106.59(13) . .
O4 P2 O5 110.40(13) . .
O6 P2 C17 109.41(15) . .
O4 P2 C17 108.26(14) . .
O5 P2 C17 106.69(15) . .
P1 O1 Mn1 140.94(14) . .
P2 O6 Mn1 146.33(14) . .
P1 O3 Mn1 131.22(13) . 2_667
C12 N2 C9 118.6(3) . .
C12 N2 Mn1 124.8(2) . .
C9 N2 Mn1 116.6(2) . .
C1 N1 C5 117.6(3) . .
C1 N1 Mn1 125.5(2) . .
C5 N1 Mn1 116.7(2) . .
C21 N3 C23 122.2(3) . .
C21 N3 C22 120.6(3) . .
C23 N3 C22 117.2(3) . .
C14 C13 C16 109.7(3) . .
C14 C13 C15 109.9(3) . .
C16 C13 C15 109.5(3) . .
C14 C13 P1 108.8(2) . .
C16 C13 P1 109.7(2) . .
C15 C13 P1 109.1(2) . .
N2 C9 C8 123.0(3) . .
N2 C9 C5 117.5(3) . .
C8 C9 C5 119.4(3) . .
N1 C1 C2 123.1(3) . .
C3 C4 C5 117.6(3) . .
C3 C4 C6 123.3(3) . .
C5 C4 C6 119.1(3) . .
C6 C7 C8 121.0(3) . .
C7 C6 C4 121.1(3) . .
C9 C8 C10 117.1(3) . .
C9 C8 C7 119.5(3) . .
C10 C8 C7 123.3(3) . .
C11 C10 C8 119.7(3) . .
C2 C3 C4 120.1(3) . .
N1 C5 C4 123.1(3) . .
N1 C5 C9 116.9(3) . .
C4 C5 C9 119.9(3) . .
C10 C11 C12 119.3(3) . .
N2 C12 C11 122.2(3) . .
C3 C2 C1 118.4(3) . .
C20 C17 C19 110.3(3) . .
C20 C17 C18 109.2(3) . .
C19 C17 C18 110.0(3) . .
C20 C17 P2 108.7(2) . .
C19 C17 P2 110.2(2) . .
C18 C17 P2 108.5(2) . .
O7 C21 N3 126.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.024(2) .
Mn1 O6 2.063(2) .
Mn1 O3 2.090(2) 2_667
Mn1 N2 2.275(3) .
Mn1 N1 2.284(3) .
P1 O1 1.498(2) .
P1 O3 1.510(2) .
P1 O2 1.579(2) .
P1 C13 1.821(3) .
P2 O6 1.495(2) .
P2 O4 1.515(2) .
P2 O5 1.573(2) .
P2 C17 1.816(3) .
O3 Mn1 2.090(2) 2_667
N2 C12 1.325(4) .
N2 C9 1.363(4) .
O7 C21 1.224(5) .
N1 C1 1.343(4) .
N1 C5 1.358(4) .
N3 C21 1.333(5) .
N3 C23 1.439(5) .
N3 C22 1.450(5) .
C13 C14 1.536(5) .
C13 C16 1.540(5) .
C13 C15 1.545(5) .
C9 C8 1.400(4) .
C9 C5 1.441(4) .
C1 C2 1.398(5) .
C4 C3 1.391(5) .
C4 C5 1.407(4) .
C4 C6 1.435(5) .
C7 C6 1.349(5) .
C7 C8 1.441(5) .
C8 C10 1.413(5) .
C10 C11 1.367(5) .
C3 C2 1.387(5) .
C11 C12 1.414(5) .
C18 C17 1.549(5) .
C20 C17 1.531(5) .
C19 C17 1.536(5) .
