Electrostatic control of the formation of heteroleptic transition metal helicates
Baylies, Christian J.; Harding, Lindsay P.; Jeffery, John C.; Moon, Ryan; Rice, Craig R.; Riis-Johannessen, T.; New Journal of Chemistry 31 (2007) 1525–; doi:10.1039/b702608k

data_7052176
_publ_section_title
;
 Electrostatic control of the formation of heteroleptic transition
 metal helicates
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1525
_journal_paper_doi               10.1039/b702608k
_journal_volume                  31
_journal_year                    2007
_chemical_formula_sum            'C79 H80.5 Ba2 Cl8 N15.5 O45 S4 Zn2'
_chemical_formula_weight         2784.35
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.4580(10)
_cell_angle_beta                 103.3020(10)
_cell_angle_gamma                110.4970(10)
_cell_formula_units_Z            2
_cell_length_a                   16.9511(3)
_cell_length_b                   18.4571(3)
_cell_length_c                   20.1644(4)
_cell_measurement_reflns_used    5770
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      140.014
_cell_measurement_theta_min      5.679
_cell_volume                     5176.27(18)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker-AXS SMART 6000'
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details      'frames, 0.3\% width'
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Frames, each covering 0.3 \% in \w'
_diffrn_measurement_specimen_support 'glass fibre'
_diffrn_radiation_collimation    'Osmic CMF12-38Cu6 (blue) mirror optics'
_diffrn_radiation_monochromator  'Osmic ConFocal MaxFlux mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         '4.8 kW rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41199
_diffrn_reflns_theta_full        70.12
_diffrn_reflns_theta_max         70.12
_diffrn_reflns_theta_min         2.50
_diffrn_source                   rotating-anode
_diffrn_source_current           120
_diffrn_source_power             4.8
_diffrn_source_size              '3 x 0.3mm'
_diffrn_source_target            Cu
_diffrn_source_type              'MAC Science M18XCE'
_diffrn_source_voltage           40
_exptl_absorpt_coefficient_mu    9.887
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.241044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2790
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.031
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1388
_refine_ls_number_reflns         17747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.096
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                13016
_reflns_number_total             17747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702608k.txt
_cod_data_source_block           craig28m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

data name '_diffrn_specimen_support' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        5176.26(16)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C79 H80.50 Ba2 Cl8 N15.50 O45 S4 Zn2'
_cod_database_code               7052176