#------------------------------------------------------------------------------
#$Date: 2015-08-08 04:53:39 +0300 (Sat, 08 Aug 2015) $
#$Revision: 153145 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/56/7035614.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_7035614
loop_
_publ_author_name
'Luan, Lindong'
'Yang, Meng'
'Bian, Yixuan'
'Lin, Zhien'
'Huang, Hui'
_publ_section_title
;
 Solvent-free synthesis of new metal phosphate-oxalates: influence of
 different metal ions on the framework structures.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13485
_journal_page_last               13489
_journal_paper_doi               10.1039/c5dt01613d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C2 H2 Co O8 P, C2 H7 N'
_chemical_formula_sum            'C4 H9 Co N O8 P'
_chemical_formula_weight         289.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-27 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3686(9)
_cell_length_b                   8.2405(5)
_cell_length_c                   13.1615(8)
_cell_measurement_reflns_used    2296
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.9370
_cell_measurement_theta_min      3.7830
_cell_volume                     1775.29(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5460
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.171
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0083(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1821
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0332P)²+3.1734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1593
_reflns_number_total             1821
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01613d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7035614--7035619.cif.'
_cod_database_code               7035614
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups
2. Restrained distances
 C4-C5
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C5')
4. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C5')=Sof(H5'A)=Sof(H5'B)=1-FVAR(1)
 Sof(H4AB)=Sof(H4AA)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4AB,H4AA), C4(H4BC,H4BD), C5(H5A,H5B), C5'(H5'A,H5'B)
5.b Me refined with riding coordinates:
 N1(H1A,H1B,H1C)
5.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.41738(2) 0.20341(5) 0.63064(3) 0.01644(15) Uani 1 1 d . . . . .
P1 P 0.43389(4) 0.56995(9) 0.72291(6) 0.0167(2) Uani 1 1 d . . . . .
O1 O 0.43234(14) 0.4507(3) 0.63740(16) 0.0271(5) Uani 1 1 d . . . . .
O2 O 0.37262(14) 0.7108(3) 0.7025(2) 0.0376(6) Uani 1 1 d . . . . .
H2 H 0.3943 0.7792 0.6662 0.056 Uiso 1 1 calc R . . . .
O3 O 0.39795(13) 0.4911(3) 0.82289(16) 0.0254(5) Uani 1 1 d . . . . .
H3 H 0.3721 0.4092 0.8081 0.038 Uiso 1 1 calc R . . . .
O4 O 0.51685(13) 0.6376(3) 0.74449(17) 0.0329(6) Uani 1 1 d . . . . .
O5 O 0.42280(12) -0.0456(2) 0.58671(16) 0.0204(5) Uani 1 1 d . . . . .
O6 O 0.49371(13) -0.2094(2) 0.48428(16) 0.0221(5) Uani 1 1 d . . . . .
O7 O 0.31739(11) 0.2286(3) 0.53163(15) 0.0227(5) Uani 1 1 d . . . . .
O8 O 0.31673(11) 0.2226(3) 0.73561(15) 0.0215(5) Uani 1 1 d . . . . .
N1 N 0.38202(18) 0.5168(4) 0.4168(2) 0.0418(8) Uani 1 1 d . . . . .
H1A H 0.3932 0.4323 0.3771 0.063 Uiso 1 1 calc R . . . .
H1B H 0.4170 0.5968 0.4036 0.063 Uiso 1 1 calc R . . . .
H1C H 0.3866 0.4875 0.4816 0.063 Uiso 1 1 calc R . . . .
C1 C 0.47618(16) -0.0735(3) 0.5206(2) 0.0180(6) Uani 1 1 d . . . . .
C2 C 0.2500 0.2500 0.5746(3) 0.0168(8) Uani 1 2 d S T P . .
C3 C 0.2500 0.2500 0.6922(3) 0.0168(8) Uani 1 2 d S T P . .
C4 C 0.2977(3) 0.5730(6) 0.3970(3) 0.0543(11) Uani 1 1 d D . . . .
H4AB H 0.2909 0.6083 0.3272 0.065 Uiso 0.395(7) 1 calc R . . A 1
H4AA H 0.2579 0.4892 0.4122 0.065 Uiso 0.395(7) 1 calc R . . A 1
H4BC H 0.2661 0.4790 0.3764 0.065 Uiso 0.605(7) 1 calc R . . A 2
H4BD H 0.2999 0.6454 0.3389 0.065 Uiso 0.605(7) 1 calc R . . A 2
C5 C 0.2915(7) 0.7101(11) 0.4686(8) 0.0415(14) Uani 0.395(7) 1 d D . . A 1
H5A H 0.3324 0.7906 0.4511 0.050 Uiso 0.395(7) 1 calc R . . A 1
H5B H 0.3035 0.6715 0.5366 0.050 Uiso 0.395(7) 1 calc R . . A 1
C5' C 0.2494(5) 0.6595(7) 0.4802(5) 0.0415(14) Uani 0.605(7) 1 d . . . A 2
H5'A H 0.1929 0.6248 0.4753 0.050 Uiso 0.605(7) 1 calc R . . A 2
H5'B H 0.2699 0.6226 0.5454 0.050 Uiso 0.605(7) 1 calc R . . A 2
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'
Co Co 0.3494 0.9721 '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'
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 Co1 O5 163.88(8) . .
O1 Co1 O6 85.72(8) . 5_656
O1 Co1 O7 91.25(9) . .
O1 Co1 O8 89.46(8) . .
O4 Co1 O1 99.56(10) 3_646 .
O4 Co1 O5 86.60(9) 3_646 .
O4 Co1 O6 102.77(9) 3_646 5_656
O4 Co1 O7 159.60(9) 3_646 .
O4 Co1 O8 84.63(8) 3_646 .
O5 Co1 O8 106.03(8) . .
O6 Co1 O5 78.37(7) 5_656 .
O6 Co1 O7 95.20(8) 5_656 .
O6 Co1 O8 171.74(8) 5_656 .
O7 Co1 O5 87.66(8) . .
O7 Co1 O8 78.18(8) . .
O1 P1 O2 110.46(14) . .
O1 P1 O3 110.49(12) . .
O1 P1 O4 113.81(14) . .
O2 P1 O3 102.14(12) . .
O4 P1 O2 109.86(14) . .
O4 P1 O3 109.46(12) . .
P1 O1 Co1 133.39(13) . .
P1 O2 H2 109.5 . .
P1 O3 H3 109.5 . .
P1 O4 Co1 137.06(14) . 3_656
C1 O5 Co1 113.16(17) . .
C1 O6 Co1 114.42(18) . 5_656
C2 O7 Co1 114.8(2) . .
C3 O8 Co1 112.8(2) . .
H1A N1 H1B 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C4 N1 H1A 109.5 . .
C4 N1 H1B 109.5 . .
C4 N1 H1C 109.5 . .
O5 C1 C1 116.9(3) . 5_656
O6 C1 O5 126.1(3) . .
O6 C1 C1 117.0(3) . 5_656
O7 C2 O7 126.3(4) 2 .
O7 C2 C3 116.87(19) . .
O7 C2 C3 116.86(19) 2 .
O8 C3 O8 125.8(4) 2 .
O8 C3 C2 117.10(19) . .
O8 C3 C2 117.10(19) 2 .
N1 C4 H4AB 111.6 . .
N1 C4 H4AA 111.6 . .
N1 C4 H4BC 107.3 . .
N1 C4 H4BD 107.3 . .
N1 C4 C5' 120.2(4) . .
H4AB C4 H4AA 109.4 . .
H4BC C4 H4BD 106.9 . .
C5 C4 N1 101.0(5) . .
C5 C4 H4AB 111.6 . .
C5 C4 H4AA 111.6 . .
C5' C4 H4BC 107.3 . .
C5' C4 H4BD 107.3 . .
C4 C5 C5 113.3(9) . 2_565
C4 C5 H5A 108.9 . .
C4 C5 H5B 108.9 . .
C5 C5 H5A 108.9 2_565 .
C5 C5 H5B 108.9 2_565 .
H5A C5 H5B 107.7 . .
C4 C5' H5'A 108.0 . .
C4 C5' H5'B 108.0 . .
C5' C5' C4 117.3(5) 2_565 .
C5' C5' H5'A 108.0 2_565 .
C5' C5' H5'B 108.0 2_565 .
H5'A C5' H5'B 107.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.054(2) .
Co1 O4 2.038(2) 3_646
Co1 O5 2.134(2) .
Co1 O6 2.100(2) 5_656
Co1 O7 2.102(2) .
Co1 O8 2.156(2) .
P1 O1 1.494(2) .
P1 O2 1.557(2) .
P1 O3 1.581(2) .
P1 O4 1.495(2) .
O2 H2 0.8200 .
O3 H3 0.8200 .
O4 Co1 2.038(2) 3_656
O5 C1 1.255(3) .
O6 Co1 2.100(2) 5_656
O6 C1 1.250(3) .
O7 C2 1.252(3) .
O8 C3 1.253(3) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N1 C4 1.479(5) .
C1 C1 1.539(5) 5_656
C2 O7 1.252(3) 2
C2 C3 1.548(6) .
C3 O8 1.253(3) 2
C4 H4AB 0.9700 .
C4 H4AA 0.9700 .
C4 H4BC 0.9700 .
C4 H4BD 0.9700 .
C4 C5 1.475(8) .
C4 C5' 1.527(7) .
C5 C5 1.51(2) 2_565
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5' C5' 1.492(12) 2_565
C5' H5'A 0.9700 .
C5' H5'B 0.9700 .
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_4
Co1 O5 C1 O6 177.5(2) . .
Co1 O5 C1 C1 -3.2(4) . 5_656
Co1 O6 C1 O5 176.9(2) 5_656 .
Co1 O6 C1 C1 -2.3(4) 5_656 5_656
Co1 O7 C2 O7 178.38(16) . 2
Co1 O7 C2 C3 -1.62(16) . .
Co1 O8 C3 O8 -174.85(15) . 2
Co1 O8 C3 C2 5.15(15) . .
O1 P1 O4 Co1 -142.7(2) . 3_656
O2 P1 O1 Co1 -127.56(18) . .
O2 P1 O4 Co1 92.9(2) . 3_656
O3 P1 O1 Co1 -15.3(2) . .
O3 P1 O4 Co1 -18.5(3) . 3_656
O4 P1 O1 Co1 108.33(19) . .
O7 C2 C3 O8 177.43(15) 2 .
O7 C2 C3 O8 -2.58(15) 2 2
O7 C2 C3 O8 177.42(15) . 2
O7 C2 C3 O8 -2.57(15) . .
N1 C4 C5 C5 -177.6(7) . 2_565
N1 C4 C5' C5' 95.1(7) . 2_565
