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_7032581
_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         'C8 H6 N2 O2, 0.5(H2 O)'
_chemical_formula_sum            'C8 H7 N2 O2.5'
_chemical_formula_weight         171.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                81.698(8)
_cell_angle_beta                 83.854(10)
_cell_angle_gamma                78.805(9)
_cell_formula_units_Z            4
_cell_length_a                   4.9524(7)
_cell_length_b                   10.9756(9)
_cell_length_c                   14.6313(15)
_cell_measurement_reflns_used    1949
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      74.1487
_cell_measurement_theta_min      3.0600
_cell_volume                     769.42(15)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
  1 omega  -48.00   36.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6873   37.0000   30.0000 84

  2 omega  -63.00  -10.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6873  -57.0000   90.0000 53

  3 omega  -51.00   39.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6873   77.0000 -150.0000 90

  4 omega -112.00  -75.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6873  -57.0000   90.0000 37

  5 omega  -33.00   16.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6873   37.0000  -30.0000 49

  6 omega   69.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6873 -125.0000 -120.0000 27

  7 omega   23.00   53.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6873  -99.0000   60.0000 30

  8 omega   61.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  -94.0000  120.0000 48

  9 omega   32.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  -94.0000   30.0000 76

 10 omega   94.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  125.0000   90.0000 84

 11 omega   82.00  137.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  -61.0000   90.0000 55

 12 omega   68.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  -45.0000    0.0000 29

 13 omega   96.00  127.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  125.0000  -30.0000 31

 14 omega   37.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  -30.0000  -30.0000 53

 15 omega   96.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  125.0000   60.0000 62

 16 omega   95.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491   31.0000 -108.0000 83

 17 omega   34.00   60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491  -61.0000   90.0000 26

 18 omega   78.00  162.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491   61.0000  150.0000 84

 19 omega   38.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7491 -125.0000  -60.0000 83
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.2631877000
_diffrn_orient_matrix_UB_12      -0.0126124000
_diffrn_orient_matrix_UB_13      -0.0425061000
_diffrn_orient_matrix_UB_21      -0.0979978000
_diffrn_orient_matrix_UB_22      0.1428379000
_diffrn_orient_matrix_UB_23      -0.0066974000
_diffrn_orient_matrix_UB_31      0.1495177000
_diffrn_orient_matrix_UB_32      0.0156710000
_diffrn_orient_matrix_UB_33      -0.0977062000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4768
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.32
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75241
_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            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2964
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0595P)^2^+0.1198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                2479
_reflns_number_total             2964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02428a2.cif
_cod_data_source_block           L4
_cod_depositor_comments
;
Adding full bibliography for 7032579--7032585.cif.

2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        769.43(15)
_cod_original_formula_moiety     '2(C8 H6 N2 O2), H2 O'
_cod_original_formula_sum        'C16 H14 N4 O5'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     342.31
_cod_database_code               7032581
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1
 0.88 with sigma of 0.02
 N13-H13
 0.88 with sigma of 0.02
 O11-H11
 0.84 with sigma of 0.02
 O25-H25B
 0.84 with sigma of 0.02
 O25-H25A
 0.84 with sigma of 0.02
 O23-H23
 0.84 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C15(H15), C17(H17), C18(H18), C19(H19)
;