Crystal structure of poly[diaqua-(μ2-4,4′-bipyridine-κ2 N:N′)-(μ2-3,4,5,6-tetrafluorophthalato-κ2 O:O′)nickel(II)], C18H12F4NiN2O6
Li, Yan-Hong; Han, Min-Le; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 563–564; doi:10.1515/ncrs-2019-0808

data_8105218
_publ_section_title
;
 Crystal structure of poly[diaqua-(\m2-4,4&#x2032;-bipyridine-\k2
 N:N&#x2032;)-(\m2-3,4,5,6-tetrafluorophthalato-\k2
 O:O&#x2032;)nickel(II)], C18H12F4NiN2O6
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              563
_journal_page_last               564
_journal_paper_doi               10.1515/ncrs-2019-0808
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         '0.5(C36 H24 F8 N4 Ni2 O12)'
_chemical_formula_sum            'C18 H12 F4 N2 Ni O6'
_chemical_formula_weight         487.01
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4650(2)
_cell_length_b                   10.6954(2)
_cell_length_c                   22.7513(5)
_cell_measurement_reflns_used    3261
_cell_measurement_temperature    293
_cell_measurement_theta_max      73.0180
_cell_measurement_theta_min      3.9020
_cell_volume                     1816.49(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -13.00  20.00   0.50    0.50    --    0.00 -57.00 -60.00   66
  2  \w    -32.00  -5.00   0.50    0.50    --    0.00 -82.00-120.00   54
  3  \w    -29.00  -3.00   0.50    0.50    --    0.00 -82.00 -30.00   52
  4  \w    -80.00 -33.00   0.50    0.50    --    0.00 -57.00 -60.00   94
  5  \w      6.00 112.00   0.50    1.54    --   95.80 -30.00-120.00  212
  6  \w     68.00 100.00   0.50    1.54    --   95.80 -30.00 -30.00   64
  7  \w     25.00  50.00   0.50    1.54    --   95.80 -30.00 -30.00   50
  8  \w      9.00 127.00   0.50    1.54    --   95.80 -82.00-150.00  236
  9  \w     95.00 138.00   0.50    1.54    --   95.80  82.00  60.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0486888000
_diffrn_orient_matrix_UB_12      0.0479675000
_diffrn_orient_matrix_UB_13      -0.0618678000
_diffrn_orient_matrix_UB_21      0.1906477000
_diffrn_orient_matrix_UB_22      0.0530373000
_diffrn_orient_matrix_UB_23      -0.0071394000
_diffrn_orient_matrix_UB_31      0.0618064000
_diffrn_orient_matrix_UB_32      -0.1250255000
_diffrn_orient_matrix_UB_33      -0.0266938000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5233
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.886
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1609
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0304
_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/[\s^2^(Fo^2^)+(0.0456P)^2^+0.9211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1435
_reflns_number_total             1609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0808_suppl.cif
_cod_data_source_block           9-25-7
_cod_database_code               8105218
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H3A-O3
 0.85 with sigma of 0.02
 H3B-O3
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.334
_oxdiff_exptl_absorpt_empirical_full_min 0.794