Recyclable scavengers for photo-cyclopropanation via an in situ crystallization process.
Lee, Haeri; Choi, Eunkyung; Noh, Tae Hwan; Jung, Ok-Sang; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18476–18483; doi:10.1039/c6dt02604d

data_7040668
_publ_section_title
;
 Recyclable scavengers for photo-cyclopropanation via an in situ
 crystallization process.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18476
_journal_page_last               18483
_journal_paper_doi               10.1039/c6dt02604d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C66 H72 N12 O33 Pd3 S3'
_chemical_formula_weight         1976.73
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-09 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   25.4354(4)
_cell_length_b                   25.4354(4)
_cell_length_c                   21.3755(6)
_cell_measurement_reflns_used    6607
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.54
_cell_measurement_theta_min      2.62
_cell_volume                     11976.3(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Breeze CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62368
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.485
_diffrn_reflns_theta_min         1.601
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             6012
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.280
_exptl_transmission_factor_max   0.002
_exptl_transmission_factor_min   0.001
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
; 
 Flack x determined using 1659 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.021(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5520
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0887P)^2^+45.9709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4112
_reflns_number_total             5520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02604d2.cif
_cod_data_source_block           1457750
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7040665--7040670.cif.
;
_cod_original_cell_volume        11976.3(5)
_cod_database_code               7040668
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.799
_shelx_res_checksum              40638