A tetrameric hetero-octanuclear cyclic helicate formed from a bridging ligand with two inequivalent binding sites
Metherell, A. J.; Ward, M. D.; RSC Advances 3 (2013) 14281–; doi:10.1039/c3ra42598c

data_7239125
_publ_section_title
;
 A tetrameric hetero-octanuclear cyclic helicate formed from a bridging
 ligand with two inequivalent binding sites
;
_journal_issue                   34
_journal_name_full               'RSC Advances'
_journal_page_first              14281
_journal_paper_doi               10.1039/c3ra42598c
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         C184H152N32O32Ti4Zn4,4(C3H7NO),4(CH4O)
_chemical_formula_sum            'C200 H196 N36 O40 Ti4 Zn4'
_chemical_formula_weight         4197.01
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.729(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   45.96(3)
_cell_length_b                   14.997(8)
_cell_length_c                   34.57(2)
_cell_measurement_reflns_used    13928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.0
_cell_volume                     20692(2)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b5 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b5 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b5 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0890
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            37310
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?sadabs?
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             8704
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         14644
_refine_ls_number_restraints     1120
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.1090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1449P)^2^+174.4715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2759
_refine_ls_wR_factor_ref         0.3000
_reflns_number_gt                10794
_reflns_number_total             14644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra42598c.txt
_cod_data_source_block           2012ncs0393
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        20692(21)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7239125