#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:42:48 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228914 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/07/7230736.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_7230736
loop_
_publ_author_name
'Jian, Fang Fang'
'Liu, E.'
'Ma, Jun Ying'
_publ_section_title
;
 Interesting fluorine anion water clusters [F−·(H2O)n] in
 metal complex crystals
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              3849
_journal_paper_doi               10.1039/C8CE00532J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'C18 H24 Co1 N12, 1(F), 2(N0.5 O1.5), 0.67(H12 O6)'
_chemical_formula_sum            'C18 H32 Co F N13 O7'
_chemical_formula_weight         620.49
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-17 deposited with the CCDC.
2018-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.9720(13)
_cell_length_b                   8.9720(13)
_cell_length_c                   21.077(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      4
_cell_volume                     1469.3(4)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRCVAX (Gabe et al., 1989)'
_computing_publication_material  'CIFTAB (Sheldrick, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9619
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.240
_diffrn_reflns_theta_min         1.932
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0398
_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)+(0.0663P)²+0.4210P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                971
_reflns_number_total             1251
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00532j2.cif
_cod_data_source_block           qj07114
_cod_depositor_comments
'Adding full bibliography for 7230735--7230737.cif.'
_cod_original_cell_volume        1469.3(5)
_cod_database_code               7230736
_shelx_shelxl_version_number     2016/6
_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   0.887
_shelx_estimated_absorpt_t_min   0.865
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.16667) H1WB(0.16667) H2WA(0.5)
3.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
Co1 Co 0.000000 0.000000 0.000000 0.0343(2) Uani 1 6 d S T P
N1 N 0.1990(2) 0.1942(2) 0.05916(7) 0.0412(4) Uani 1 1 d . . .
N2 N 0.3765(2) 0.3193(3) 0.13862(9) 0.0516(5) Uani 1 1 d . . .
H2 H 0.429895 0.332304 0.173879 0.062 Uiso 1 1 calc R . .
C1 C 0.3998(3) 0.4451(3) 0.09763(13) 0.0650(7) Uani 1 1 d . . .
H1 H 0.476224 0.562297 0.102262 0.078 Uiso 1 1 calc R . .
C2 C 0.2914(3) 0.3682(3) 0.04894(11) 0.0553(6) Uani 1 1 d . . .
H2A H 0.280697 0.424554 0.013691 0.066 Uiso 1 1 calc R . .
C3 C 0.2552(3) 0.1715(3) 0.11398(10) 0.0452(5) Uani 1 1 d . . .
H3 H 0.214883 0.064770 0.133189 0.054 Uiso 1 1 calc R . .
F1 F 1.000000 1.000000 0.250000 0.0924(14) Uani 1 6 d S T P
N3 N 0.666667 0.333333 0.250000 0.0433(9) Uani 1 6 d S T P
O1 O 0.8285(2) 0.4393(3) 0.250000 0.0461(5) Uani 1 2 d S T P
O1W O 0.333333 0.666667 0.250000 0.167(5) Uani 1 6 d S T P
H1WA H 0.333333 0.666667 0.209670 0.200 Uiso 0.5 3 d RS T P
H1WB H 0.370820 0.596410 0.250000 0.200 Uiso 0.3333 2 d RS T P
O2W O 0.6703(4) 0.7314(4) 0.250000 0.1146(14) Uani 1 2 d S T P
H2WA H 0.627028 0.707096 0.212980 0.137 Uiso 0.5 1 d R . .
H2WB H 0.660338 0.632076 0.250000 0.137 Uiso 1 2 d RS T 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'
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'
F F 0.0171 0.0103 '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
N1 Co1 N1 90.02(6) 7 9
N1 Co1 N1 89.98(6) 3 8
N1 Co1 N1 90.02(6) 2 .
N1 Co1 N1 89.98(6) 7 3
N1 Co1 N1 180.0 7 .
N1 Co1 N1 180.00(10) 9 3
N1 Co1 N1 90.02(6) 9 8
N1 Co1 N1 89.98(6) 7 2
N1 Co1 N1 180.00(9) 2 8
N1 Co1 N1 89.98(6) 9 2
N1 Co1 N1 89.98(6) 9 .
N1 Co1 N1 90.02(6) 3 2
N1 Co1 N1 89.98(6) 8 .
N1 Co1 N1 90.02(6) 7 8
N1 Co1 N1 90.02(6) 3 .
C2 N1 Co1 127.86(14) . .
C3 N1 Co1 127.40(14) . .
C3 N1 C2 104.72(17) . .
C3 N2 C1 106.90(18) . .
C2 C1 N2 106.8(2) . .
C1 C2 N1 109.6(2) . .
N1 C3 N2 111.95(19) . .
O1 N3 O1 120.002(1) 3_665 2_655
O1 N3 O1 120.000(1) . 2_655
O1 N3 O1 119.998(1) . 3_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.1604(16) 7
Co1 N1 2.1604(16) .
Co1 N1 2.1604(16) 8
Co1 N1 2.1604(16) 9
Co1 N1 2.1604(16) 3
Co1 N1 2.1604(16) 2
N1 C2 1.370(3) .
N1 C3 1.317(3) .
N2 C1 1.352(3) .
N2 C3 1.330(3) .
C1 C2 1.343(3) .
N3 O1 1.2775(18) .
N3 O1 1.2775(18) 2_655
N3 O1 1.2775(18) 3_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
N2 H2 N3 0.86 2.66 3.4607(18) 155.8 .
N2 H2 O1 0.86 1.90 2.757(2) 173.3 2_655
O1W H1WB O2W 0.85 2.33 2.779(3) 113.3 .
O2W H2WB O1 0.85 1.90 2.715(3) 161.1 2_655
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
Co1 N1 C2 C1 178.38(17)
Co1 N1 C3 N2 -178.60(13)
N2 C1 C2 N1 0.3(3)
C1 N2 C3 N1 0.3(3)
C2 N1 C3 N2 -0.1(2)
C3 N1 C2 C1 -0.1(3)
C3 N2 C1 C2 -0.3(3)
