Crystal structure of diaqua-bis(1,10-phenanthroline κ2 N,N′)nickel(II) trifluoroacetate- trifluoroacetic acid (1/1), C30H21F9N4NiO8
Zhang, Lan; Wang, Qiang; Ding, Wu-Xiu; Hao, Hui-Min; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 869–871; doi:10.1515/ncrs-2019-0052

data_8105877
_publ_section_title
;
 Crystal structure of diaqua-bis(1,10-phenanthroline \k2
 N,N&#x2032;)nickel(II) trifluoroacetate- trifluoroacetic acid (1/1),
 C30H21F9N4NiO8
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              869
_journal_page_last               871
_journal_paper_doi               10.1515/ncrs-2019-0052
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C24 H20 N4 Ni O2, 2(C2 H0.5 F3 O2), C2 F3 O2'
_chemical_formula_sum            'C30 H21 F9 N4 Ni O8'
_chemical_formula_weight         795.22
_chemical_name_systematic
;
diaqua-bis(1,10-phenanthroline)-nickel(II) trifluoroacetate
trifluoroacetic acid
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 116.10(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0630(11)
_cell_length_b                   9.6250(10)
_cell_length_c                   18.196(2)
_cell_measurement_reflns_used    1124
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     1582.7(5)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009) [12]'
_computing_data_collection       'Bruker SMART [13]'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009) [12]'
_computing_molecular_graphics    'Diamond 4.0 [14]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [15]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [16]'
_computing_structure_solution    'ShelXS (Sheldrick, 2008) [17]'
_diffrn_ambient_temperature      297
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7825
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.116
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  0.9976
_exptl_absorpt_correction_T_min  0.8524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0511
_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/[\s^2^(Fo^2^)+(0.0541P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1773
_reflns_number_total             2789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0052_suppl.cif
_cod_data_source_block           a
_cod_database_code               8105877
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid body (RIGU) restrains
 F4, F5, C16, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H1A(0.5) F4(0.5) F5(0.5) F6(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
4.b Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;