A total synthesis of milbemycin G: approaches to the C1-C10-fragment and completion of the synthesis.
Bailey, Simon; Helliwell, Madeleine; Teerawutgulrag, Aphiwat; Thomas, Eric J.; Organic & biomolecular chemistry 3 (2005) 3654–3677; doi:10.1039/b508675b

data_7150262
_publ_section_title
;
 A total synthesis of milbemycin G: approaches to the C1-C10-fragment
 and completion of the synthesis.
;
_journal_issue                   20
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3654
_journal_page_last               3677
_journal_paper_doi               10.1039/b508675b
_journal_volume                  3
_journal_year                    2005
_chemical_formula_moiety         'C27 H33 Cl O9 Si '
_chemical_formula_sum            'C27 H33 Cl O9 Si'
_chemical_formula_weight         565.09
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      169
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_audit_creation_date             19105-06-15
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             ?
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.153(1)
_cell_length_b                   14.153
_cell_length_c                   25.881(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      22.8
_cell_measurement_theta_min      14.8
_cell_volume                     4489.6(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01566
_diffrn_orient_matrix_UB_12      -0.07615
_diffrn_orient_matrix_UB_13      0.00649
_diffrn_orient_matrix_UB_21      -0.08002
_diffrn_orient_matrix_UB_22      -0.02620
_diffrn_orient_matrix_UB_23      0.00015
_diffrn_orient_matrix_UB_31      -0.00299
_diffrn_orient_matrix_UB_32      -0.01308
_diffrn_orient_matrix_UB_33      -0.03809
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.08139
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            2592
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        5.41
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1788.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.499
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     0
_refine_ls_number_reflns         1156
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0907
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0954
_reflns_number_observed          1156
_reflns_number_total             2292
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b508675b.txt
_cod_data_source_block           S400-4
_cod_depositor_comments
;
 Homogenising atom site labels in order to relate data from different loops.

 Antanas Vaitkus,
 2018-08-08

 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'hexgonal' was replaced with
'hexagonal' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00022|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4489.3(7)
_cod_original_sg_symbol_H-M      'P 61 '
_cod_original_formula_sum        'C27 H33 Cl O9 Si '
_cod_database_code               7150262