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_7032584
_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         'C36 H32 Cu3 N10 O16, 2.25(C6 H6), 2(H2 O)'
_chemical_formula_sum            'C49.5 H49.5 Cu3 N10 O18'
_chemical_formula_weight         1263.11
_chemical_name_systematic
;
 ? 
;
_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
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Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                105.934(4)
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_cell_formula_units_Z            1
_cell_length_a                   10.2213(6)
_cell_length_b                   11.4215(5)
_cell_length_c                   14.0872(7)
_cell_measurement_reflns_used    9142
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      73.7592
_cell_measurement_theta_min      3.4044
_cell_volume                     1467.04(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
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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)'
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_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0(10)
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;
  1 omega -114.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega -104.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6512  -57.0000 -150.0000 94

  3 omega  -42.00   36.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6512   37.0000 -180.0000 78

  4 omega -103.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6512  -57.0000  120.0000 91

  5 omega   26.00   97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6512 -128.0000   19.0000 71

  6 omega    4.00   70.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6512  -99.0000   90.0000 66

  7 omega   34.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega    7.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   88.0000  -21.0000 25

  9 omega   13.00   45.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   82.0000 -140.0000 32

 10 omega   12.00   37.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   84.0000   33.0000 25

 11 omega   17.00   45.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000  -72.0000 28

 12 omega   17.00   42.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   81.0000   76.0000 25

 13 omega  -55.00  -28.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000  150.0000 27

 14 omega  -54.00  -28.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 15 omega  -54.00  -28.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 16 omega   33.00   61.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 17 omega   32.00   61.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   75.0000   84.0000 29

 18 omega  103.00  141.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   75.0000   84.0000 38

 19 omega   31.00   59.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   75.0000  131.0000 28

 20 omega  109.00  137.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   75.0000  -25.0000 28

 21 omega   96.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   75.0000  131.0000 27

 22 omega   37.00   75.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  171.0000 38

 23 omega  101.00  146.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   30.0000 45

 24 omega   35.00   75.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   30.0000 40

 25 omega   34.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  -72.0000 33

 26 omega   82.00  142.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  171.0000 60

 27 omega   39.00   80.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   75.0000  -10.0000 41

 28 omega   88.00  120.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   77.0000 -125.0000 32

 29 omega   42.00   80.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   77.0000 -125.0000 38

 30 omega   30.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -94.0000   30.0000 76

 31 omega   75.00  170.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   77.0000  -30.0000 95

 32 omega   75.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   77.0000  120.0000 102

 33 omega  128.00  168.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  125.0000   30.0000 40

 34 omega   78.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   61.0000   90.0000 27

 35 omega   74.00  147.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   77.0000 -120.0000 73

 36 omega   78.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   61.0000  -60.0000 30

 37 omega   32.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -94.0000  120.0000 71

 38 omega   82.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 39 omega   80.00  170.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   61.0000   30.0000 90

 40 omega   74.00  101.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   77.0000   30.0000 27

 41 omega   74.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   77.0000    0.0000 26

 42 omega   59.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853  -45.0000  150.0000 39

 43 omega   75.00  143.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   77.0000  -60.0000 68

 44 omega   33.00  118.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 45 omega  113.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 46 omega   76.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 47 omega   74.00  100.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 48 omega   74.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 49 omega   74.00  101.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 50 omega   81.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
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 51 omega   74.00  172.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7853   77.0000   60.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_12      0.0459974000
_diffrn_orient_matrix_UB_13      0.0643834000
_diffrn_orient_matrix_UB_21      -0.1202720000
_diffrn_orient_matrix_UB_22      -0.0389059000
_diffrn_orient_matrix_UB_23      -0.0996133000
_diffrn_orient_matrix_UB_31      -0.0547346000
_diffrn_orient_matrix_UB_32      -0.1353358000
_diffrn_orient_matrix_UB_33      0.0061135000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
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_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22189
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         73.92
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79362
_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    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0996P)^2^+1.8571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                4919
_reflns_number_total             5737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02428a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7032579--7032585.cif.'
_cod_original_cell_volume        1467.04(13)
_cod_original_formula_sum        'C49.50 H49.50 Cu3 N10 O18'
_cod_database_code               7032584
_reflns_odcompleteness_completeness 98.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H37A,H37B} of O37, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H36A,H36B} of O36, All O(H) groups
2. Restrained distances
 O27-H27
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: N31(0.5) O33(0.5) N34(0.5) O35(0.5) C41(0.75) H41(0.75) C42(0.75)
 H42(0.75) C43(0.75) H43(0.75) C44(0.75) H44(0.75) C45(0.75) H45(0.75)
 C46(0.75) H46(0.75) C38(0.75) H38(0.75) C39(0.75) H39(0.75) C40(0.75)
 H40(0.75) O36(0.5) H36A(0.5) H36B(0.5) O37(0.5) H37A(0.5) H37B(0.5)
5.a Free rotating group:
 O36(H36A,H36B), O37(H37A,H37B)
5.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B)
5.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C6(H6), C8(H8), C9(H9), C11(H11), N16(H16), C18(H18), C20(H20),
 C21(H21), C23(H23), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C38(H38), C39(H39), C40(H40)
5.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C)
;