Crystal structure of dimethanolo-bis[μ-(2-(2-(5-(pyridin-2-yl)-1H-1,2,4-triazol-3-yl)phenoxy)benzoato)-κ5 O,O′,N:N′,N′′]dicopper(II) — methanol (1/2), C46H48Cu2N8O12
Qiang Li, Guo; Hong He, Jia; Yun Hui, Cai; Xu, Qiang; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 1127–1129; doi:10.1515/ncrs-2016-0087

data_8107121
_publ_section_title
;
 Crystal structure of
 dimethanolo-bis[\m-(2-(2-(5-(pyridin-2-yl)-1H-1,2,4-triazol-3-yl)phenoxy)benzoato)-\k5
 O,O&#x2032;,N:N&#x2032;,N&#x2032;&#x2032;]dicopper(II) --- methanol
 (1/2), C46H48Cu2N8O12
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1127
_journal_page_last               1129
_journal_paper_doi               10.1515/ncrs-2016-0087
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C42 H32 Cu2 N8 O8, 4(C H4 O)'
_chemical_formula_sum            'C46 H48 Cu2 N8 O12'
_chemical_formula_weight         1032.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5638(9)
_cell_length_b                   20.2142(19)
_cell_length_c                   12.0825(11)
_cell_measurement_reflns_used    7630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.509
_cell_measurement_theta_min      2.362
_cell_volume                     2328.0(4)
_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      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16067
_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    0.985
_exptl_absorpt_correction_T_max  0.8273
_exptl_absorpt_correction_T_min  0.8273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'blue block'
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0340P)^2^+1.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                3617
_reflns_number_total             4102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2016-0087_suppl.cif
_cod_data_source_block           a
_cod_database_code               8107121
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 C21-H4
 1.897125 with sigma of 0.02
 Cu1-H4
 2.908057 with sigma of 0.02
3. Rigid bond restraints
 N1, Cu1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Riding coordinates:
 O6(H6), O5(H5)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C1(H1), C15(H15), C11(H11), C10(H10), C18(H18), C2(H2), C16(H16),
 C4(H4A), C9(H9), C3(H3), C17(H17)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'