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_7040669
_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_moiety
'C114 H120 N24 O18 Pd3, 6(N O3), 12(C2 H6 S O), 4(H2 O)'
_chemical_formula_sum            'C138 H200 N30 O52 Pd3 S12'
_chemical_formula_weight         3815.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-17 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.933(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3794(5)
_cell_length_b                   72.214(2)
_cell_length_c                   15.4212(5)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.05
_cell_measurement_theta_min      2.16
_cell_volume                     19116.9(10)
_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 0.748
_diffrn_measured_fraction_theta_max 0.726
_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  0.0758
_diffrn_reflns_av_unetI/netI     0.1320
_diffrn_reflns_Laue_measured_fraction_full 0.748
_diffrn_reflns_Laue_measured_fraction_max 0.726
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       87
_diffrn_reflns_limit_k_min       -79
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            108728
_diffrn_reflns_point_group_measured_fraction_full 0.748
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.128
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             7936
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.270
_exptl_transmission_factor_max   0.004
_exptl_transmission_factor_min   0.001
_refine_diff_density_max         1.776
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1875
_refine_ls_number_reflns         27257
_refine_ls_number_restraints     1547
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.1288
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1627P)^2^+200.5496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3483
_refine_ls_wR_factor_ref         0.3732
_refine_special_details
;
 The structure contains large solvent accessible voids. According 
to the TGA and proton NMR spectra, the asymmetric unit of 3.(NO3)6 
contains about twelve dimethyl sulfoxide and four water molecules. 
Except refined six dimethyl sulfoxide, SQUEEZE procedure has been 
used in order to remove electronic density peaks from disordered 
solvent molecules. 
;
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14485
_reflns_number_total             27257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02604d2.cif
_cod_data_source_block           1457751
_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_database_code               7040669
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.820
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              16337
_platon_squeeze_void_probe_radius 1.20