New structural motifs in chromium(iii) calix[4 and 6]arene chemistry
Redshaw, Carl; Homden, Damien; Hughes, David L.; Wright, Joseph A.; Elsegood, Mark R. J.; Dalton Transactions  (2009) 1231–1242; doi:10.1039/b813313a

data_7000497
_publ_section_title
;
 New structural motifs in chromium(iii) calix[4 and 6]arene chemistry
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1231
_journal_page_last               1242
_journal_paper_doi               10.1039/b813313a
_journal_year                    2009
_chemical_formula_moiety         'C50 H64 Cl2 Cr Li N2 O4, 2(C2 H3 N)'
_chemical_formula_sum            'C54 H70 Cl2 Cr Li N4 O4'
_chemical_formula_weight         968.98
_chemical_name_common            'Compound 6'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 108.3226(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1176(2)
_cell_length_b                   21.8758(4)
_cell_length_c                   18.4573(3)
_cell_measurement_reflns_used    57012
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     5411.24(15)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
'DENZO (Otwinowski and Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al</i>, 1993)'
_computing_publication_material
;
Bruker SHELXTL, PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\F & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66013
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         12367
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0562P)^2^+3.7497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                9300
_reflns_number_total             12367
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b813313a.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7000497