Crystal structure of bis(1-ethyl-6-fluoro-4-oxido-7-(piperazin-1-ium-1-yl)-1,8-naphthyridin-1-ium-3-carboxylate-κ2 O,O′)copper(II) benzene-1, 4-dicarboxylate dihydrate, C38H42F2CuN8O12
Cui, Kuo; Wang, Liang-Liang; Zhang, Wen-Wei; Liu, Fu-Xin; Zhang, Wen-Jun; Fan, Zhuo-Wen; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 1219–1220; doi:10.1515/ncrs-2016-0140

data_8107150
_publ_section_title
;
 Crystal structure of
 bis(1-ethyl-6-fluoro-4-oxido-7-(piperazin-1-ium-1-yl)-1,8-naphthyridin-1-ium-3-carboxylate-\k2
 O,O&#x2032;)copper(II) benzene-1, 4-dicarboxylate dihydrate,
 C38H42F2CuN8O12
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1219
_journal_page_last               1220
_journal_paper_doi               10.1515/ncrs-2016-0140
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C30 H34 Cu F2 N8 O6, C8 H4 O4, 2(H2 O)'
_chemical_formula_sum            'C38 H42 Cu F2 N8 O12'
_chemical_formula_weight         904.34
_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                95.014(2)
_cell_angle_beta                 92.041(2)
_cell_angle_gamma                103.223(2)
_cell_formula_units_Z            1
_cell_length_a                   5.4709(2)
_cell_length_b                   10.4100(4)
_cell_length_c                   17.3373(6)
_cell_measurement_reflns_used    5812
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.24
_cell_volume                     955.96(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13821
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.18
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.8687
_exptl_absorpt_correction_T_min  0.8527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             469
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3380
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.3636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                3071
_reflns_number_total             3380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2016-0140_suppl.cif
_cod_data_source_block           Cu-en-bdc
_cod_database_code               8107150
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All H(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 H6A_$1-O6_$1
 0.9 with sigma of 0.02
 H6B_$1-O6_$1
 0.9 with sigma of 0.02
 H6A_$1-H6B_$1
 1.25 with sigma of 0.02
 H6B_$1-H6B_$2
 2.15 with sigma of 0.02
 H6A_$1-O6_$1 \\sim O6_$1-H6B_$1
 with sigma of 0.02
 H6A_$1-O6_$1 \\sim O6_$1-H6B_$1
 with sigma of 0.0001
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C16(H16), C18(H18)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'