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_7000493
_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
'C98 H120 Cr2 K N5 O16, C100 H123 Cr2 K N6, C2 H3 N'
_chemical_formula_sum            'C200 H246 Cr4 K2 N12 O16'
_chemical_formula_weight         3360.29
_chemical_name_common            'Compound 2'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                102.3503(16)
_cell_angle_beta                 98.4355(17)
_cell_angle_gamma                94.8829(17)
_cell_formula_units_Z            2
_cell_length_a                   17.1144(15)
_cell_length_b                   23.373(2)
_cell_length_c                   24.339(2)
_cell_measurement_reflns_used    13091
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.14
_cell_volume                     9339.1(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1441
_diffrn_reflns_av_sigmaI/netI    0.2194
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54754
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS v2.01; Sheldrick, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2277
_refine_ls_number_reflns         24403
_refine_ls_number_restraints     912
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.2020
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1268P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2665
_reflns_number_gt                10448
_reflns_number_total             24403
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b813313a.txt
_cod_data_source_block           2
_cod_original_cell_volume        9339.2(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000493