Discrete and polymeric Cu(ii) complexes featuring substituted indazole ligands: their synthesis and structural chemistry.
Hawes, Chris S.; Kruger, Paul E.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16450–16458; doi:10.1039/c4dt02428a

data_7032585
_publ_section_title
;
 Discrete and polymeric Cu(ii) complexes featuring substituted indazole
 ligands: their synthesis and structural chemistry.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16450
_journal_page_last               16458
_journal_paper_doi               10.1039/c4dt02428a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C16 H10 Cu N4 O4, 0.5(C2 H2 O2), H2 O'
_chemical_formula_sum            'C17 H16 Cu N4 O6'
_chemical_formula_weight         435.88
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 124.140(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.730(2)
_cell_length_b                   4.5836(2)
_cell_length_c                   17.8406(13)
_cell_measurement_reflns_used    2520
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      73.6582
_cell_measurement_theta_min      2.9902
_cell_volume                     1741.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      120.0(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -48.00   29.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563   37.0000 -180.0000 77

  2 omega  -79.00   44.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563    0.0000  120.0000 123

  3 omega  -45.00    7.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.6563   37.0000    0.0000 52

  4 omega   30.00   78.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       39.6563 -125.0000   90.0000 48

  5 omega   30.00   97.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       39.6563 -125.0000  -90.0000 67

  6 omega   33.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  120.0000 43

  7 omega   51.00  111.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -77.0000    0.0000 60

  8 omega   73.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000    0.0000 25

  9 omega   95.00  160.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   61.0000  -60.0000 65

 10 omega  126.00  168.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   45.0000  150.0000 42

 11 omega   94.00  138.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000 -120.0000 44

 12 omega   55.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000  -90.0000 41

 13 omega   39.00  119.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000   30.0000 80

 14 omega   77.00  171.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000 -120.0000 94

 15 omega   33.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -120.0000 54

 16 omega   41.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000 -180.0000 52

 17 omega   31.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000  120.0000 61

 18 omega   31.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -30.0000 60

 19 omega   55.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000 -120.0000 65
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0251861000
_diffrn_orient_matrix_UB_12      -0.2079084000
_diffrn_orient_matrix_UB_13      0.0813072000
_diffrn_orient_matrix_UB_21      0.0677229000
_diffrn_orient_matrix_UB_22      0.0901391000
_diffrn_orient_matrix_UB_23      0.0352295000
_diffrn_orient_matrix_UB_31      -0.0035803000
_diffrn_orient_matrix_UB_32      0.2482970000
_diffrn_orient_matrix_UB_33      0.0550589000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5385
_diffrn_reflns_theta_full        73.82
_diffrn_reflns_theta_max         73.82
_diffrn_reflns_theta_min         4.15
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         1742
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0560P)^2^+5.7306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                1640
_reflns_number_total             1742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02428a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7032579--7032585.cif.'
_cod_original_cell_volume        1741.5(2)
_cod_database_code               7032585
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H14-O14
 0.85 with sigma of 0.02
 H15-O15
 0.85 with sigma of 0.02
 H3-N3
 0.88 with sigma of 0.02
3. Others
 Fixed Sof: O15(0.5) H15(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8)
;