#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:25:00 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180504 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/73/7217360.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_7217360
loop_
_publ_author_name
'Tang, Si-Fu'
'Li, Liang-Jun'
'Lv, Xiao-Xia'
'Wang, Chao'
'Zhao, Xue-Bo'
_publ_section_title
;
 Tuning the structure of metal phosphonates using uncoordinating methyl
 group: syntheses, structures and properties of a series of metal
 diphosphonates
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              7043
_journal_paper_doi               10.1039/C4CE00375F
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C8 H18 Mn O10 P2'
_chemical_formula_weight         391.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.064(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.825(4)
_cell_length_b                   8.3912(16)
_cell_length_c                   9.2901(18)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.998
_cell_measurement_theta_min      2.659
_cell_volume                     1463.8(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.973
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4587
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.659
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1250
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0517P)²+2.6453P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1148
_reflns_number_total             1250
_reflns_threshold_expression     'I > 2σ(I)'
_cod_duplicate_entry             7216041
_cod_data_source_file            c4ce00375f2.cif
_cod_data_source_block           a
_cod_database_code               7217360
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn1 Mn 0.5000 0.33867(7) 0.2500 0.0224(2) Uani 1 2 d S T P
O1W O 0.42780(15) 0.1450(3) 0.1577(3) 0.0599(8) Uani 1 1 d . . .
H1W H 0.4037 0.1882 0.0877 0.072 Uiso 1 1 d . U .
H2W H 0.4387 0.0515 0.1878 0.072 Uiso 1 1 d . U .
O1 O 0.58045(10) 0.5111(3) 0.32625(19) 0.0296(5) Uani 1 1 d . . .
O2 O 0.54913(9) 0.6635(2) 0.5495(2) 0.0261(4) Uani 1 1 d . . .
O3 O 0.61634(10) 0.4017(2) 0.5684(2) 0.0282(5) Uani 1 1 d . . .
H3A H 0.6067 0.4158 0.6522 0.042 Uiso 1 1 calc R U .
P1 P 0.60214(3) 0.56056(8) 0.47953(7) 0.0217(2) Uani 1 1 d . . .
C1 C 0.75035(16) 0.4360(4) 0.3617(4) 0.0391(8) Uani 1 1 d . . .
H1A H 0.7981 0.4140 0.3373 0.059 Uiso 1 1 calc R U .
H1B H 0.7190 0.4360 0.2755 0.059 Uiso 1 1 calc R U .
H1C H 0.7354 0.3554 0.4265 0.059 Uiso 1 1 calc R U .
C2 C 0.74803(14) 0.5970(3) 0.4336(3) 0.0249(6) Uani 1 1 d . . .
C3 C 0.68631(14) 0.6641(3) 0.4849(3) 0.0224(6) Uani 1 1 d . . .
C4 C 0.68966(14) 0.8142(3) 0.5494(3) 0.0250(6) Uani 1 1 d . . .
H4A H 0.6482 0.8568 0.5826 0.030 Uiso 1 1 calc R U .
O2W O 0.4962(6) -0.1550(9) 0.2906(10) 0.108(3) Uani 0.5 1 d . U P
O2W' O 0.4856(6) 0.0975(12) -0.1016(12) 0.122(3) Uani 0.5 1 d . U P
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'
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
O2 Mn1 O2 179.03(10) 6_565 5_666
O2 Mn1 O1 93.21(7) 6_565 2_655
O2 Mn1 O1 87.43(7) 5_666 2_655
O2 Mn1 O1 87.43(7) 6_565 .
O2 Mn1 O1 93.21(7) 5_666 .
O1 Mn1 O1 96.67(11) 2_655 .
O2 Mn1 O1W 87.06(9) 6_565 .
O2 Mn1 O1W 92.24(9) 5_666 .
O1 Mn1 O1W 88.19(10) 2_655 .
O1 Mn1 O1W 172.85(9) . .
O2 Mn1 O1W 92.24(9) 6_565 2_655
O2 Mn1 O1W 87.06(9) 5_666 2_655
O1 Mn1 O1W 172.85(9) 2_655 2_655
O1 Mn1 O1W 88.19(10) . 2_655
O1W Mn1 O1W 87.47(16) . 2_655
P1 O1 Mn1 128.64(10) . .
P1 O2 Mn1 135.55(11) . 5_666
O2 P1 O1 114.97(12) . .
O2 P1 O3 110.60(10) . .
O1 P1 O3 106.55(11) . .
O2 P1 C3 108.67(12) . .
O1 P1 C3 109.65(11) . .
O3 P1 C3 106.02(11) . .
C4 C2 C3 117.3(2) 7_666 .
C4 C2 C1 118.7(2) 7_666 .
C3 C2 C1 124.0(2) . .
C4 C3 C2 119.7(2) . .
C4 C3 P1 117.37(19) . .
C2 C3 P1 122.9(2) . .
C2 C4 C3 123.1(2) 7_666 .
O2W O2W O2W' 155.0(7) 2_655 6_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.1376(18) 6_565
Mn1 O2 2.1376(18) 5_666
Mn1 O1 2.1764(19) 2_655
Mn1 O1 2.1764(19) .
Mn1 O1W 2.249(3) .
Mn1 O1W 2.249(3) 2_655
O1 P1 1.5114(19) .
O2 P1 1.5021(19) .
O2 Mn1 2.1376(18) 5_666
O3 P1 1.581(2) .
P1 C3 1.805(3) .
C1 C2 1.509(4) .
C2 C4 1.389(4) 7_666
C2 C3 1.405(4) .
C3 C4 1.394(4) .
C4 C2 1.389(4) 7_666
O2W O2W 0.778(17) 2_655
O2W O2W' 1.141(12) 6_556
O2W' O2W 1.141(12) 6
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
O3 H3A O1 0.82 1.83 2.638(2) 168.1 6_566
O1W H1W O3 0.85 2.32 3.081(4) 149.8 2_655
O1W H2W O1W 0.85 2.91 3.109(6) 95.4 2_655
