#------------------------------------------------------------------------------
#$Date: 2017-04-04 05:52:55 +0300 (Tue, 04 Apr 2017) $
#$Revision: 194679 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/79/7227971.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_7227971
loop_
_publ_author_name
'Zhang, Li'
'Li, Sanying'
'Liu, Lei'
'Dong, Jinxiang'
'Lin, Zhi'
_publ_section_title
;
 Four new zinc (II) diphosphonates obtained via an ionothermal route:
 crystal structures and phase transformation behaviour
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00400A
_journal_year                    2017
_chemical_formula_moiety         '0.5(C16 H24 O16 P4 Zn4)'
_chemical_formula_sum            'C8 H12 O8 P2 Zn2'
_chemical_formula_weight         428.86
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2016-12-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-17 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.259(2)
_cell_length_b                   5.8452(6)
_cell_length_c                   4.9451(4)
_cell_measurement_reflns_used    1267
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.266
_cell_measurement_theta_min      3.662
_cell_volume                     643.40(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1519
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            2895
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         3.661
_exptl_absorpt_coefficient_mu    4.010
_exptl_absorpt_correction_T_max  0.8561
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.030(8)
_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   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0580
_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)+(0.0928P)²+0.4595P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                538
_reflns_number_total             607
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00400a2.cif
_cod_data_source_block           1502886
_cod_database_code               7227971
_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.
;
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C2(0.5) H3A(0.5) C4(0.5) H4(0.5)
3.a Riding coordinates:
 O3(H3), C1(H1A,H1B), C3(H3A), C4(H4)
;
_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, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zn1 Zn 0.26170(4) 0.2500 -0.0913(2) 0.0266(6) Uani 1 2 d S T P
P1 P 0.17476(9) 0.2500 0.3612(4) 0.0217(7) Uani 1 2 d S T P
O1 O 0.2043(2) 0.0347(8) 0.2200(10) 0.0432(14) Uani 1 1 d . . .
O2 O 0.1826(3) 0.2500 0.6712(11) 0.0280(14) Uani 1 2 d S T P
O3 O 0.3366(3) 0.2500 0.2092(14) 0.0353(15) Uani 1 2 d S T P
H3 H 0.3317 0.1332 0.3092 0.042 Uiso 1 1 d R . .
C1 C 0.0965(4) 0.2500 0.272(2) 0.070(4) Uani 1 2 d S T P
H1A H 0.0957 0.2015 0.0866 0.084 Uiso 0.5 1 d R . .
H1B H 0.0854 0.4087 0.2701 0.084 Uiso 0.5 1 d R . .
C2 C 0.0462(5) 0.145(2) 0.390(2) 0.024(3) Uani 0.5 1 d . . .
C3 C 0.0138(4) 0.2500 0.621(2) 0.047(3) Uani 1 2 d S T P
H3A H 0.0200 0.4011 0.6918 0.057 Uiso 0.5 1 d R . .
C4 C 0.0326(5) -0.073(2) 0.271(2) 0.025(2) Uani 0.5 1 d . . .
H4 H 0.0545 -0.1122 0.1109 0.031 Uiso 0.5 1 d 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'
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'
Zn Zn 0.2839 1.4301 '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 Zn1 O1 108.4(3) 2_554 7_665
O1 Zn1 O1 64.3(2) 8_565 .
O1 Zn1 O1 93.64(11) 7_665 8_565
O1 Zn1 O1 158.0(2) 7_665 .
O1 Zn1 O1 93.64(11) 2_554 .
O1 Zn1 O1 158.0(2) 2_554 8_565
O1 Zn1 O2 93.11(16) 7_665 1_554
O1 Zn1 O2 93.11(16) 2_554 1_554
O1 Zn1 O3 91.57(16) 7_665 .
O1 Zn1 O3 91.57(16) 2_554 .
O2 Zn1 O1 84.96(17) 1_554 .
O2 Zn1 O1 84.96(17) 1_554 8_565
O2 Zn1 O3 172.0(2) 1_554 .
O3 Zn1 O1 88.26(18) . .
O3 Zn1 O1 88.26(18) . 8_565
O1 P1 O1 105.3(4) . 8_565
O1 P1 C1 107.2(3) . .
O1 P1 C1 107.2(3) 8_565 .
O2 P1 O1 113.0(2) . 8_565
O2 P1 O1 113.0(2) . .
O2 P1 C1 110.7(4) . .
Zn1 O1 Zn1 121.9(2) 2 .
P1 O1 Zn1 126.7(3) . 2
P1 O1 Zn1 95.1(2) . .
P1 O2 Zn1 130.2(3) . 1_556
Zn1 O3 H3 106.9 . .
P1 C1 H1A 104.7 . .
P1 C1 H1B 104.6 . .
H1A C1 H1B 105.7 . .
C2 C1 P1 132.2(7) 8_565 .
C2 C1 P1 132.2(7) . .
C2 C1 H1A 120.6 8_565 .
C2 C1 H1A 104.5 . .
C2 C1 H1B 102.9 . .
C2 C1 H1B 51.3 8_565 .
C2 C1 C2 52.1(11) . 8_565
C1 C2 C3 121.6(10) . .
C1 C2 C4 113.0(10) . .
C2 C2 C1 63.9(6) 8_565 .
C2 C2 C3 65.5(5) 8_565 .
C2 C2 C4 152.6(6) 8_565 .
C4 C2 C3 125.4(10) . .
C2 C3 C2 49.0(10) 8_565 .
C2 C3 H3A 126.3 . .
C2 C3 H3A 80.2 8_565 .
C2 C3 C4 108.0(7) 8_565 4_556
C2 C3 C4 149.5(9) . 4_556
C2 C3 C4 108.0(7) . 5_556
C2 C3 C4 149.5(9) 8_565 5_556
C4 C3 H3A 125.7 5_556 .
C4 C3 H3A 50.0 4_556 .
C4 C3 C4 83.6(10) 5_556 4_556
C2 C4 C3 126.3(10) . 5_556
C2 C4 H4 116.4 . .
C3 C4 H4 117.3 5_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.052(4) 2_554
Zn1 O1 2.363(5) .
Zn1 O1 2.363(5) 8_565
Zn1 O1 2.052(4) 7_665
Zn1 O2 2.116(6) 1_554
Zn1 O3 2.233(6) .
P1 O1 1.582(4) 8_565
P1 O1 1.582(4) .
P1 O2 1.543(6) .
P1 C1 1.797(10) .
O1 Zn1 2.052(4) 2
O2 Zn1 2.116(6) 1_556
O3 H3 0.8500 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 C2 1.404(15) .
C1 C2 1.404(15) 8_565
C2 C2 1.23(3) 8_565
C2 C3 1.487(15) .
C2 C4 1.430(19) .
C3 C2 1.487(15) 8_565
C3 H3A 0.9600 .
C3 C4 1.557(14) 4_556
C3 C4 1.557(14) 5_556
C4 C3 1.557(14) 5_556
C4 H4 0.9600 .
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
P1 C1 C2 C2 116.3(9) . 8_565
P1 C1 C2 C3 83.7(11) . .
P1 C1 C2 C4 -93.7(11) . .
O1 P1 O1 Zn1 133.7(2) 8_565 2
O1 P1 O1 Zn1 -3.1(4) 8_565 .
O1 P1 O2 Zn1 -59.8(2) 8_565 1_556
O1 P1 O2 Zn1 59.8(2) . 1_556
O1 P1 C1 C2 160.0(9) . 8_565
O1 P1 C1 C2 87.3(10) . .
O1 P1 C1 C2 -160.0(9) 8_565 .
O1 P1 C1 C2 -87.3(10) 8_565 8_565
O2 P1 O1 Zn1 9.8(5) . 2
O2 P1 O1 Zn1 -127.0(2) . .
O2 P1 C1 C2 36.3(9) . 8_565
O2 P1 C1 C2 -36.3(9) . .
C1 P1 O1 Zn1 -112.4(4) . 2
C1 P1 O1 Zn1 110.8(3) . .
C1 P1 O2 Zn1 180.000(0) . 1_556
C1 C2 C3 C2 32.1(11) . 8_565
C1 C2 C3 C4 -171.3(9) . 5_556
C1 C2 C3 C4 80(2) . 4_556
C1 C2 C4 C3 170.4(9) . 5_556
C2 C1 C2 C3 -32.6(12) 8_565 .
C2 C1 C2 C4 150.0(7) 8_565 .
C2 C2 C3 C4 48.0(15) 8_565 4_556
C2 C2 C3 C4 156.6(9) 8_565 5_556
C2 C2 C4 C3 -112.2(13) 8_565 5_556
C3 C2 C4 C3 -6.9(19) . 5_556
C4 C2 C3 C2 -150.8(9) . 8_565
C4 C2 C3 C4 5.8(16) . 5_556
C4 C2 C3 C4 -102.8(15) . 4_556
