A [Cu~3~(μ~3~-O)]–pyrazolate metallacycle with terminal nitrate ligands exhibiting point group symmetry 3
Mathivathanan, Logesh; Cruz, Raquel; Raptis, Raphael G.; Acta Crystallographica Section E 72 (2016) 492–494; doi:10.1107/S2056989016003741

data_2241604
_publ_section_title
;
 A [Cu~3~(\m~3~-O)]--pyrazolate metallacycle with terminal nitrate ligands
 exhibiting point group symmetry 3
;
_journal_coeditor_code           WM4004
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              492
_journal_page_last               494
_journal_paper_doi               10.1107/S2056989016003741
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'(C36 H30 P2 N) [Cu3 (C3 H2 Cl1 N2)3 (N O3)3 O]  N O3, H2 O1'
_chemical_formula_moiety
'3(C36 H30 P2 N +), C9 H6 Cl3 Cu3 N9 O10 2-. N O3 -, H2 O1'
_chemical_formula_sum            'C117 H98 Cl3 Cu3 N13 O14 P6'
_chemical_formula_weight         2390.85
_chemical_name_systematic
;Tris[bis(triphenylphosphoranylidene)ammonium]
tris(\m~2~-4-chloropyrazolato-\k^2^<i>N</i>:<i>N</i>')-\m~3~-oxido-tris[(nitrato-\k^2^<i>O</i>,<i>O</i>')cuprate(II)] nitrate monohydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.038(2)
_cell_length_b                   23.038(2)
_cell_length_c                   18.4214(17)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.32
_cell_volume                     8467.3(13)
_computing_cell_refinement
;
SAINT (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2005)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30414
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.358
_diffrn_reflns_theta_min         2.322
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.9049
_exptl_absorpt_correction_T_min  0.8401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2005)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       polygon
_exptl_crystal_F_000             3687
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.289
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2750 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7675
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.1352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                6428
_reflns_number_total             7675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4004sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-21
;
_cod_original_cell_volume        8466.9(17)
_cod_database_code               2241604
_cod_database_fobs_code          2241604
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.905
_shelx_hkl_checksum              10190
_shelx_res_checksum              65324