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_7000492
_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         'C104 H132 Cl2 Cr2 Li4 N4 O11, 2.25(C2 H3 N)'
_chemical_formula_sum            'C108.5 H138.75 Cl2 Cr2 Li4 N6.25 O11'
_chemical_formula_weight         1909.17
_chemical_name_common            'Compound 1'
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6211(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8446(7)
_cell_length_b                   36.770(2)
_cell_length_c                   24.6560(14)
_cell_measurement_reflns_used    41766
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.21
_cell_volume                     10587.3(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      160(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66796
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS v2.01; Sheldrick, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4062
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         3.887
_refine_diff_density_min         -2.061
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1314
_refine_ls_number_reflns         18473
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1020
_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^)+(0.1259P)^2^+60.4193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2674
_refine_ls_wR_factor_ref         0.2880
_reflns_number_gt                13989
_reflns_number_total             18473
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b813313a.txt
_cod_data_source_block           1
_cod_original_cell_volume        10587.3(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C108.50 H138.75 Cl2 Cr2 Li4 N6.25 O11'
_cod_database_code               7000492