Crystal structure of bis(biphenyl-2,2′-dicarboxylato-κ2 O:O′)-bis(1-cyclopropyl-6-fluoro-4-oxo-7-(1-piperazinyl)-1,4-dihydroquinoline-3-carboxylato-κ2 O,O′)dizinc(II)2.5 hydrate, C62H57N6Zn2O16.5F2
Hu, Yong-Jun; Zhu, Ling; An, Zhe; Zhou, Tian; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 1111–1113; doi:10.1515/ncrs-2016-0080

data_8107116
_publ_section_title
;
 Crystal structure of bis(biphenyl-2,2&#x2032;-dicarboxylato-\k2
 O:O&#x2032;)-bis(1-cyclopropyl-6-fluoro-4-oxo-7-(1-piperazinyl)-1,4-dihydroquinoline-3-carboxylato-\k2
 O,O&#x2032;)dizinc(II)2.5 hydrate, C62H57N6Zn2O16.5F2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1111
_journal_page_last               1113
_journal_paper_doi               10.1515/ncrs-2016-0080
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C62 H52 F2 N6 O14 Zn2, 2.5(H2 O)'
_chemical_formula_sum            'C62 H57 F2 N6 O16.5 Zn2'
_chemical_formula_weight         1318.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                112.473(3)
_cell_angle_beta                 105.835(4)
_cell_angle_gamma                91.309(4)
_cell_formula_units_Z            1
_cell_length_a                   10.026(4)
_cell_length_b                   12.064(4)
_cell_length_c                   13.385(5)
_cell_measurement_reflns_used    8785
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.720
_cell_measurement_theta_min      2.300
_cell_volume                     1424.5(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11392
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.8361
_exptl_absorpt_correction_T_min  0.8361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadsbs
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             681
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.6381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                4645
_reflns_number_total             4995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2016-0080_suppl.cif
_cod_data_source_block           a
_cod_original_cell_volume        1424.4(9)
_cod_original_formula_sum        'C62 H57 F2 N6 O16.50 Zn2'
_cod_database_code               8107116
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O9(0.25) H9A(0.25) H9B(0.25)
3.a Riding coordinates:
 O8(H8A,H8B), O9(H9A,H9B)
3.b Ternary CH refined with riding coordinates:
 C4(H4)
3.c Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C17(H17A,H17B), C14(H14A,H14B), C16(H16A,H16B), C5(H5A,H5B),
 C15(H15A,H15B), C6(H6A,H6B)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C13(H13), C26(H26), C29(H29), C20(H20), C28(H28), C23(H23),
 C27(H27), C21(H21), C22(H22)
;
_olex2_submission_special_instructions 'No special instructions were received'