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_7032582
_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         '2(C24 H18 Cu N7 O3), 2(N O3), 3(H2 O)'
_chemical_formula_sum            'C48 H42 Cu2 N16 O15'
_chemical_formula_weight         1210.06
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 99.328(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2872(2)
_cell_length_b                   15.9102(5)
_cell_length_c                   21.2623(6)
_cell_measurement_reflns_used    2585
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.4065
_cell_measurement_theta_min      2.7750
_cell_volume                     2432.57(12)
_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  'XLMP (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 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -49.00   34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9012   37.0000   60.0000 83

  2 omega  -70.00    4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9012   77.0000 -150.0000 74

  3 omega  -69.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9012   57.0000  150.0000 102

  4 omega   51.00   77.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -45.0000  -60.0000 26

  5 omega   33.00   89.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -45.0000 -180.0000 56

  6 omega   34.00   94.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -45.0000    0.0000 60

  7 omega   96.00  178.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   30.0000  120.0000 82

  8 omega   30.00   82.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -30.0000  -60.0000 52

  9 omega  143.00  169.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  125.0000   30.0000 26

 10 omega   41.00  116.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853 -125.0000    0.0000 75

 11 omega   44.00   83.00   1.0000   82.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -30.0000 -150.0000 39
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.2110275000
_diffrn_orient_matrix_UB_12      -0.0126617000
_diffrn_orient_matrix_UB_13      -0.0036039000
_diffrn_orient_matrix_UB_21      0.0308271000
_diffrn_orient_matrix_UB_22      -0.0264668000
_diffrn_orient_matrix_UB_23      0.0707030000
_diffrn_orient_matrix_UB_31      -0.0200874000
_diffrn_orient_matrix_UB_32      0.0922297000
_diffrn_orient_matrix_UB_33      0.0196295000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9042
_diffrn_reflns_theta_full        73.57
_diffrn_reflns_theta_max         73.57
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97178
_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            green
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0747P)^2^+3.1349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                3688
_reflns_number_total             4759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02428a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7032579--7032585.cif.'
_cod_original_cell_volume        2432.58(13)
_cod_database_code               7032582
_chemical_oxdiff_formula         C20H20N4O4CU1
_reflns_odcompleteness_completeness 99.93
_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,H) groups
2. Restrained distances
 N37-O39 = N37-O36 = N37-O38
 1.25 with sigma of 0.02
 N41-O43 = N41-O40 = N41-O42
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N41) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O36)
\\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O42) \\sim Ueq,
Uanis(N37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: N41(0.5) O40(0.5) O42(0.5) O43(0.5) N37(0.5) O36(0.5) O38(0.5)
 O39(0.5) O44(0.5) H44A(0.5) H44B(0.5) O45(0.5) H45A(0.5) H45B(0.5) O46(0.5)
 H46A(0.5) H46B(0.5)
5.a Free rotating group:
 O44(H44A,H44B), O45(H45A,H45B), O46(H46A,H46B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C27(H27), C28(H28),
  C29(H29), C30(H30)
;