Synthesis and characterization of a Bi10O8(OAr)16 oxo-cluster supported by p-tert-butylcalix[5]arene ligands.
Mendoza-Espinosa, Daniel; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13399–13405; doi:10.1039/c6dt02068b

data_7040045
_publ_section_title
;
 Synthesis and characterization of a Bi10O8(OAr)16 oxo-cluster supported
 by p-tert-butylcalix[5]arene ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13399
_journal_page_last               13405
_journal_paper_doi               10.1039/c6dt02068b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C248 H288 Bi10 O28, 4(C4 H7 O)'
_chemical_formula_sum            'C264 H316 Bi10 O32'
_chemical_formula_weight         6090.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-24
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.05.11 svn.r3296 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-07-21 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.749(6)
_cell_length_b                   23.749(6)
_cell_length_c                   24.831(4)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     14005(5)
_computing_cell_refinement       'Gemini Agilen'
_computing_data_collection       'Gemini Agilent'
_computing_data_reduction        CrisAlisPro
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    CrisAlisPro
_diffrn_ambient_temperature      213.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'phi and omega scans'
_diffrn_measurement_method       'not recorded'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1990
_diffrn_reflns_av_unetI/netI     0.1045
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40456
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.319
_diffrn_reflns_theta_max         23.319
_diffrn_reflns_theta_min         1.715
_exptl_absorpt_coefficient_mu    6.316
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5972
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         6.268
_refine_diff_density_min         -2.492
_refine_diff_density_rms         0.263
_refine_ls_abs_structure_details
;
 Flack x determined using 3538 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         10143
_refine_ls_number_restraints     758
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1325P)^2^+481.5425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1957
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8516
_reflns_number_total             10143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02068b2.cif
_cod_data_source_block           shelx_sq
_cod_depositor_comments          'Adding full bibliography for 7040045.cif.'
_cod_original_cell_volume        14005(7)
_cod_database_code               7040045
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C57, C62, C61, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C59 \\sim C60 \\sim C61 \\sim C62: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C46, Bi1, O6, O7, O1, Bi2, Bi3, C1, C2, C6, C3, C55, C5, C11, C4, C49, C12,
 C7, C48, C50, C13, C17, C8, C9, C10, C47, O5, C45, C14, O2, C16, C51, C44, C15,
  C18, C56, C22, C52, C53, C54, C38, C19, C20, C21, C57, C23, C37, C39, C58,
 C62, C24, C28, C36, O4, C34, C59, C61, C25, O3, C27, C35, C40, C33, C60, C0AA,
 C29, C41, C42, C43, C30, C1AA, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C63, C66, H63, C64, C65, H66A, H66B, H64A, H64B, H65A, H65B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C51, C52, C53, C54} sigma for 1-2: 0.02, 1-3: 0.04
as
{C40, C41, C42, C43}
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B), C55(H55A,
 H55B), C56(H56A,H56B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B)
6.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C30(H30A,H30B,H30C), C1AA(H1AA,H1AB,H1AC), C32(H32A,H32B,H32C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15), C24(H24), C0AA(H0AA), C35(H35), C37(H37),
 C46(H46), C48(H48), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
6.d Fitted hexagon refined as free rotating group:
 C57(C58,C59,C60,C61,C62)
6.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              50810
_shelx_fab_checksum              93309
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'