#------------------------------------------------------------------------------
#$Date: 2020-04-05 12:57:33 +0200 (dom 05 de abr de 2020) $
#$Revision: 250323 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/18/7701871.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_7701871
loop_
_publ_author_name
'Liu, Sheng-Bo'
'Bao, Song-Song'
'Zheng, Li-Min'
_publ_section_title
;
 Polar layered coordination polymers incorporating
 triazacyclononane-triphosphonate metalloligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3758
_journal_page_last               3765
_journal_paper_doi               10.1039/c9dt03858b
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C9 H20 Cl Fe N3 O10 P3 Zn2'
_chemical_formula_sum            'C9 H20 Cl Fe N3 O10 P3 Zn2'
_chemical_formula_weight         645.23
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-01 deposited with the CCDC.	2019-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.9323(4)
_cell_length_b                   8.9323(4)
_cell_length_c                   13.2617(7)
_cell_measurement_reflns_used    5015
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.633
_cell_volume                     916.34(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.633
_exptl_absorpt_coefficient_mu    3.845
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.338
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1418
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0284
_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)+(0.0352P)²+1.2297P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                1365
_reflns_number_total             1418
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03858b2.cif
_cod_data_source_block           1_D
_cod_depositor_comments
'Adding full bibliography for 7701871--7701872.cif.'
_cod_original_cell_volume        916.34(10)
_cod_database_code               7701871
_shelx_shelxl_version_number     2018/3
_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_min   0.447
_shelx_estimated_absorpt_t_max   0.655
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+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
Fe1 Fe 1.000000 0.000000 0.69365(10) 0.0077(3) Uani 1 3 d S T P
Zn1 Zn 0.333333 -0.333333 0.75711(8) 0.0108(2) Uani 1 3 d S T P
Zn2 Zn 0.666667 0.333333 0.85519(8) 0.0143(3) Uani 1 3 d S T P
P1 P 0.67314(17) 0.02027(17) 0.73499(14) 0.0106(3) Uani 1 1 d . . .
Cl1 Cl 0.333333 -0.333333 0.9222(2) 0.0305(7) Uani 1 3 d S T P
C1 C 0.8007(7) 0.1743(7) 0.6378(4) 0.0125(11) Uani 1 1 d . . .
H1A H 0.723524 0.190991 0.591271 0.015 Uiso 1 1 calc R U .
H1B H 0.881179 0.287178 0.668926 0.015 Uiso 1 1 calc R U .
C2 C 1.0577(7) 0.2607(7) 0.5356(4) 0.0142(11) Uani 1 1 d . U .
H2A H 1.113028 0.354108 0.586353 0.017 Uiso 1 1 calc R U .
H2B H 1.023741 0.306139 0.477238 0.017 Uiso 1 1 calc R U .
C3 C 0.7946(8) -0.0214(8) 0.5021(4) 0.0161(12) Uani 1 1 d . U .
H3A H 0.863013 0.004154 0.439299 0.019 Uiso 1 1 calc R U .
H3B H 0.690713 -0.012601 0.487088 0.019 Uiso 1 1 calc R U .
N1 N 0.9004(5) 0.1097(6) 0.5804(3) 0.0114(9) Uani 1 1 d . U .
O1 O 0.7890(5) -0.0549(5) 0.7658(3) 0.0120(8) Uani 1 1 d . . .
O2 O 0.5023(5) -0.1181(5) 0.6903(4) 0.0166(8) Uani 1 1 d . . .
O3 O 0.6467(6) 0.1181(5) 0.8192(3) 0.0179(9) Uani 1 1 d . . .
O1W O 0.666667 0.333333 1.0067(6) 0.0251(18) Uani 1 3 d S T P
H1WB H 0.573410 0.247860 1.028009 0.038 Uiso 0.3333 1 d R U P
H1WC H 0.752140 0.325540 1.028009 0.038 Uiso 0.3333 1 d R 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
Zn Zn 0.2839 1.4301 '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'
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 Fe1 O1 97.87(15) 5_765 .
O1 Fe1 O1 97.87(15) 5_765 3_645
O1 Fe1 O1 97.87(15) . 3_645
O1 Fe1 N1 162.60(16) 5_765 3_645
O1 Fe1 N1 99.05(16) . 3_645
O1 Fe1 N1 83.79(15) 3_645 3_645
O1 Fe1 N1 83.79(16) 5_765 5_765
O1 Fe1 N1 162.60(16) . 5_765
O1 Fe1 N1 99.04(16) 3_645 5_765
N1 Fe1 N1 78.85(18) 3_645 5_765
O1 Fe1 N1 99.05(16) 5_765 .
O1 Fe1 N1 83.79(15) . .
O1 Fe1 N1 162.60(16) 3_645 .
N1 Fe1 N1 78.85(18) 3_645 .
N1 Fe1 N1 78.85(18) 5_765 .
O2 Zn1 O2 101.22(17) . 3_545
O2 Zn1 O2 101.22(17) . 5_655
O2 Zn1 O2 101.22(17) 3_545 5_655
O2 Zn1 Cl1 116.82(14) . .
O2 Zn1 Cl1 116.82(14) 3_545 .
O2 Zn1 Cl1 116.82(14) 5_655 .
O3 Zn2 O3 113.91(10) . 3_655
O3 Zn2 O3 113.91(10) . 5_665
O3 Zn2 O3 113.91(10) 3_655 5_665
O3 Zn2 O1W 104.55(13) . .
O3 Zn2 O1W 104.55(13) 3_655 .
O3 Zn2 O1W 104.55(13) 5_665 .
O3 P1 O2 112.0(2) . .
O3 P1 O1 112.9(2) . .
O2 P1 O1 111.6(2) . .
O3 P1 C1 108.0(2) . .
O2 P1 C1 109.5(3) . .
O1 P1 C1 102.4(2) . .
N1 C1 P1 109.9(3) . .
N1 C1 H1A 109.7 . .
P1 C1 H1A 109.7 . .
N1 C1 H1B 109.7 . .
P1 C1 H1B 109.7 . .
H1A C1 H1B 108.2 . .
N1 C2 C3 109.9(4) . 5_765
N1 C2 H2A 109.7 . .
C3 C2 H2A 109.7 5_765 .
N1 C2 H2B 109.7 . .
C3 C2 H2B 109.7 5_765 .
H2A C2 H2B 108.2 . .
N1 C3 C2 112.1(4) . 3_645
N1 C3 H3A 109.2 . .
C2 C3 H3A 109.2 3_645 .
N1 C3 H3B 109.2 . .
C2 C3 H3B 109.2 3_645 .
H3A C3 H3B 107.9 . .
C1 N1 C3 113.0(4) . .
C1 N1 C2 109.1(4) . .
C3 N1 C2 111.7(4) . .
C1 N1 Fe1 106.1(3) . .
C3 N1 Fe1 111.2(3) . .
C2 N1 Fe1 105.3(3) . .
P1 O1 Fe1 122.4(2) . .
P1 O2 Zn1 125.9(3) . .
P1 O3 Zn2 144.1(3) . .
Zn2 O1W H1WB 109.5 . .
Zn2 O1W H1WC 109.5 . .
H1WB O1W H1WC 109.5 . .
Zn2 O1W H1WB 109.468(2) . 5_665
H1WB O1W H1WB 109.5 . 5_665
H1WC O1W H1WB 109.5 . 5_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.945(4) 5_765
Fe1 O1 1.945(4) .
Fe1 O1 1.945(4) 3_645
Fe1 N1 2.208(4) 3_645
Fe1 N1 2.208(4) 5_765
Fe1 N1 2.208(4) .
Zn1 O2 1.964(4) .
Zn1 O2 1.964(4) 3_545
Zn1 O2 1.964(4) 5_655
Zn1 Cl1 2.189(3) .
Zn2 O3 1.901(4) .
Zn2 O3 1.901(4) 3_655
Zn2 O3 1.901(4) 5_665
Zn2 O1W 2.009(8) .
P1 O3 1.507(4) .
P1 O2 1.524(4) .
P1 O1 1.544(4) .
P1 C1 1.813(6) .
C1 N1 1.490(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 N1 1.501(6) .
C2 C3 1.507(8) 5_765
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 N1 1.495(7) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
O1W H1WB 0.8490 .
O1W H1WC 0.8491 .
O1W H1WB 0.8490 5_665
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
_geom_hbond_publ_flag
C1 H1A Cl1 0.99 2.75 3.650(6) 151.9 2_554 yes
C2 H2A O2 0.99 2.48 3.296(7) 139.3 5_765 yes
C2 H2B O3 0.99 2.46 3.325(7) 146.1 6_664 yes
C3 H3A O1 0.99 2.58 3.466(7) 148.3 6_664 yes
O1W H1WB O2 0.85 2.38 3.000(8) 130.7 4_655 yes
O1W H1WC O2 0.85 2.38 3.000(8) 130.7 6_665 yes
C1 H1A Cl1 0.99 2.75 3.650(6) 151.9 2_554 yes
C2 H2A O2 0.99 2.48 3.296(7) 139.3 5_765 yes
C2 H2B O3 0.99 2.46 3.325(7) 146.1 6_664 yes
C3 H3A O1 0.99 2.58 3.466(7) 148.3 6_664 yes
O1W H1WB O2 0.85 2.38 3.000(8) 130.7 4_655 yes
O1W H1WC O2 0.85 2.38 3.000(8) 130.7 6_665 yes
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
O3 P1 C1 N1 152.7(3) .
O2 P1 C1 N1 -85.1(4) .
O1 P1 C1 N1 33.4(4) .
P1 C1 N1 C3 80.4(5) .
P1 C1 N1 C2 -154.7(3) .
P1 C1 N1 Fe1 -41.7(4) .
C2 C3 N1 C1 -102.3(6) 3_645
C2 C3 N1 C2 134.3(5) 3_645
C2 C3 N1 Fe1 16.9(6) 3_645
C3 C2 N1 C1 164.7(4) 5_765
C3 C2 N1 C3 -69.7(6) 5_765
C3 C2 N1 Fe1 51.2(5) 5_765
O3 P1 O1 Fe1 -122.9(3) .
O2 P1 O1 Fe1 109.9(3) .
C1 P1 O1 Fe1 -7.1(3) .
O3 P1 O2 Zn1 -70.3(3) .
O1 P1 O2 Zn1 57.4(4) .
C1 P1 O2 Zn1 170.0(3) .
O2 P1 O3 Zn2 -107.5(5) .
O1 P1 O3 Zn2 125.5(5) .
C1 P1 O3 Zn2 13.0(6) .
