One-step assembly of Re(i) tricarbonyl 2-pyridyltetrazolato metallacalix[3]arene with aqua emission and reversible three-electron oxidation.
Wright, Phillip J.; Muzzioli, Sara; Skelton, Brian W.; Raiteri, Paolo; Lee, Jackson; Koutsantonis, George; Silvester, Debbie S.; Stagni, Stefano; Massi, Massimiliano; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8188–8191; doi:10.1039/c3dt50988e

data_7021545
_publ_section_title
;
 One-step assembly of Re(i) tricarbonyl 2-pyridyltetrazolato
 metallacalix[3]arene with aqua emission and reversible three-electron
 oxidation.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8188
_journal_page_last               8191
_journal_paper_doi               10.1039/c3dt50988e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C27 H12 N15 O9 Re3, 2(C H2 Cl2)'
_chemical_formula_sum            'C29 H16 Cl4 N15 O9 Re3'
_chemical_formula_weight         1418.97
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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             2012-11-01T11:34:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.082(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2409(2)
_cell_length_b                   24.9665(5)
_cell_length_c                   17.3333(3)
_cell_measurement_reflns_used    19188
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      31.5981
_cell_measurement_theta_min      2.8385
_cell_volume                     4430.98(15)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0188175
_diffrn_orient_matrix_UB_12      -0.0188316
_diffrn_orient_matrix_UB_13      -0.0287551
_diffrn_orient_matrix_UB_21      -0.0069899
_diffrn_orient_matrix_UB_22      -0.0198895
_diffrn_orient_matrix_UB_23      0.0288266
_diffrn_orient_matrix_UB_31      -0.0663438
_diffrn_orient_matrix_UB_32      0.0074375
_diffrn_orient_matrix_UB_33      0.0043198
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83582
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    8.48
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.094
_refine_diff_density_min         -1.964
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.32
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         10698
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.32
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+107.8012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                10227
_reflns_number_total             10698
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt50988e.txt
_cod_data_source_block           mxm75
_cod_database_code               7021545