#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:32:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180186 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/82/7108269.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_7108269
loop_
_publ_author_name
'Bryan Yonemoto'
'Zhuo-jia Lin'
'Feng Jiao'
_publ_section_title
;
 A general synthetic method for MPO4 (M = Co, Fe, Mn) frameworks using
 deep-eutectic solvents
;
_journal_name_full               Chem.Commun.
_journal_page_first              9132
_journal_paper_doi               10.1039/c2cc34020h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C9 H44 Co10 N10 O40 P10'
_chemical_formula_weight         1831.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   9.880(2)
_cell_length_b                   9.880(2)
_cell_length_c                   13.333(3)
_cell_measurement_reflns_used    952
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      3.06
_cell_volume                     1301.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0097
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14337
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    3.521
_exptl_absorpt_correction_T_max  0.6479
_exptl_absorpt_correction_T_min  0.6348
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1270
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0609P)²+6.9168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                1268
_reflns_number_total             1270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34020h.txt
_cod_data_source_block           feng3
_cod_original_cell_volume        1301.6(5)
_cod_original_sg_symbol_H-M      P-42(1)c
_cod_database_code               7108269
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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 0.64064(7) 0.39604(7) 0.19823(6) 0.0179(2) Uani 1 1 d .
Co2 Co 0.5000 0.5000 0.5000 0.0180(3) Uani 1 4 d S
P1 P 0.38461(15) 0.32716(14) 0.32088(11) 0.0192(3) Uani 1 1 d .
P2 P 0.5000 0.5000 0.0000 0.0188(6) Uani 1 4 d S
O1 O 0.5588(5) 0.3858(5) 0.0648(3) 0.0285(10) Uani 1 1 d .
O2 O 0.8165(4) 0.3101(4) 0.1788(4) 0.0291(10) Uani 1 1 d .
O3 O 0.6765(5) 0.5830(4) 0.2380(3) 0.0295(10) Uani 1 1 d .
O4 O 0.5366(4) 0.3050(5) 0.3012(4) 0.0301(10) Uani 1 1 d .
O5 O 0.3668(5) 0.3931(5) 0.4247(3) 0.0320(10) Uani 1 1 d .
N1 N 0.5000 0.0000 0.7399(12) 0.092(5) Uani 1 2 d S
H1A H 0.4467 0.0515 0.7792 0.110 Uiso 0.50 1 d PR
H1B H 0.4497 -0.0521 0.6989 0.110 Uiso 0.50 1 d PR
N2Q N 0.170(2) 0.316(3) 0.5583(17) 0.083(10) Uani 0.38 1 d PD
H2QC H 0.1703 0.2847 0.6218 0.125 Uiso 0.38 1 d PR
H2QD H 0.1618 0.2454 0.5156 0.125 Uiso 0.38 1 d PR
H2QE H 0.2487 0.3590 0.5460 0.125 Uiso 0.38 1 d PR
N3Q N -0.1712(13) 0.3101(12) 0.4357(9) 0.017(3) Uani 0.38 1 d PDU
H3QC H -0.2188 0.2671 0.3878 0.025 Uiso 0.38 1 d PR
H3QD H -0.1173 0.2504 0.4675 0.025 Uiso 0.38 1 d PR
H3QE H -0.2285 0.3477 0.4802 0.025 Uiso 0.38 1 d PR
C1Q C 0.035(4) 0.434(3) 0.5401(17) 0.082(11) Uani 0.38 1 d PDU
H1QA H 0.0464 0.5029 0.5901 0.098 Uiso 0.38 1 d PR
H1QB H -0.0444 0.3842 0.5583 0.098 Uiso 0.38 1 d PR
C2Q C 0.0000 0.5000 0.4499(12) 0.098(10) Uani 0.75 2 d SPDU
H2QA H 0.0822 0.5226 0.4154 0.118 Uiso 0.38 1 d PR
H2QB H -0.0461 0.5829 0.4655 0.118 Uiso 0.38 1 d PR
C3Q C -0.0831(19) 0.4184(18) 0.3871(11) 0.030(4) Uani 0.38 1 d PDU
H3QA H -0.1424 0.4786 0.3515 0.036 Uiso 0.38 1 d PR
H3QB H -0.0255 0.3763 0.3382 0.036 Uiso 0.38 1 d PR
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
O4 Co1 O2 111.39(19) . .
O4 Co1 O3 110.1(2) . .
O2 Co1 O3 106.6(2) . .
O4 Co1 O1 113.7(2) . .
O2 Co1 O1 103.0(2) . .
O3 Co1 O1 111.7(2) . .
O5 Co2 O5 118.5(3) . 2_665
O5 Co2 O5 105.14(13) . 4_656
O5 Co2 O5 105.14(13) 2_665 4_656
O5 Co2 O5 105.14(13) . 3_566
O5 Co2 O5 105.14(13) 2_665 3_566
O5 Co2 O5 118.5(3) 4_656 3_566
O2 P1 O4 107.9(3) 6_455 .
O2 P1 O3 110.1(3) 6_455 2_665
O4 P1 O3 110.0(3) . 2_665
O2 P1 O5 109.0(3) 6_455 .
O4 P1 O5 109.0(3) . .
O3 P1 O5 110.9(3) 2_665 .
O1 P2 O1 111.6(3) 3_565 4_655
O1 P2 O1 108.44(16) 3_565 2_665
O1 P2 O1 108.44(16) 4_655 2_665
O1 P2 O1 108.44(16) 3_565 .
O1 P2 O1 108.44(16) 4_655 .
O1 P2 O1 111.6(3) 2_665 .
P2 O1 Co1 129.0(3) . .
P1 O2 Co1 141.7(3) 6 .
P1 O3 Co1 131.9(3) 2_665 .
P1 O4 Co1 124.9(3) . .
P1 O5 Co2 127.6(3) . .
C2Q C1Q C1Q 58.3(14) . 2_565
C2Q C1Q N2Q 127(2) . .
C1Q C1Q N2Q 158(3) 2_565 .
C1Q C2Q C1Q 63(3) 2_565 .
C1Q C2Q C3Q 128.3(16) 2_565 .
C1Q C2Q C3Q 112.4(13) . .
C1Q C2Q C3Q 112.4(13) 2_565 2_565
C1Q C2Q C3Q 128.3(16) . 2_565
C3Q C2Q C3Q 107.9(19) . 2_565
C2Q C3Q N3Q 118.5(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O4 1.936(4) .
Co1 O2 1.951(4) .
Co1 O3 1.954(4) .
Co1 O1 1.957(5) .
Co2 O5 1.963(5) .
Co2 O5 1.963(5) 2_665
Co2 O5 1.963(5) 4_656
Co2 O5 1.963(5) 3_566
P1 O2 1.514(4) 6_455
P1 O4 1.540(4) .
P1 O3 1.541(4) 2_665
P1 O5 1.541(4) .
P2 O1 1.535(4) 3_565
P2 O1 1.535(4) 4_655
P2 O1 1.535(4) 2_665
P2 O1 1.535(4) .
O2 P1 1.514(4) 6
O3 P1 1.541(4) 2_665
N2Q C1Q 1.79(5) .
N3Q C3Q 1.52(2) .
C1Q C2Q 1.41(2) .
C1Q C1Q 1.49(7) 2_565
C2Q C1Q 1.41(2) 2_565
C2Q C3Q 1.423(17) .
C2Q C3Q 1.423(17) 2_565
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
N1 H1A O2 0.90 1.96 2.825(8) 161.0 3_566
N1 H1A O4 0.90 2.65 3.144(6) 115.3 7
N2Q H2QC O3 0.90 2.07 2.89(3) 151.6 8_445
N2Q H2QD O1 0.90 1.97 2.804(18) 154.2 6_455
N2Q H2QE O5 0.90 2.02 2.74(2) 136.1 .
N3Q H3QD O1 0.90 2.24 2.985(14) 139.7 6_455
N3Q H3QE O5 0.90 2.07 2.930(13) 159.2 4_556
