Clathrochelates meet phosphorus: thiophosphorylation of Fe(ii) dichloroclathrochelate precursor, synthesis of N,S-donor macrobicyclic ligands and their Pd(ii) complexes as potent catalysts of Suzuki cross-coupling reaction.
Artyushin, Oleg I.; Odinets, Irina L.; Matveeva, Ekaterina V.; Vologzhanina, Anna V.; Varzatskii, Oleg A.; Lyubimov, Sergey E.; Voloshin, Yan Z.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 9677–9689; doi:10.1039/c3dt53590h

data_7030963
_publ_section_title
;
 Clathrochelates meet phosphorus: thiophosphorylation of Fe(ii)
 dichloroclathrochelate precursor, synthesis of N,S-donor macrobicyclic
 ligands and their Pd(ii) complexes as potent catalysts of Suzuki
 cross-coupling reaction.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9677
_journal_page_last               9689
_journal_paper_doi               10.1039/c3dt53590h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C48 H36 B2 Cl F2 Fe N8 O6 P Pd S, C H2 Cl2, 0.5(H2 O) '
_chemical_formula_sum            'C49 H39 B2 Cl3 F2 Fe N8 O6.5 P Pd S'
_chemical_formula_weight         1235.13
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.304(8)
_cell_length_b                   12.319(7)
_cell_length_c                   25.949(16)
_cell_measurement_reflns_used    945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      2.28
_cell_volume                     5514(5)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1609
_diffrn_reflns_av_sigmaI/netI    0.1492
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41061
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.9581
_exptl_absorpt_correction_T_min  0.7941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.357
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         10808
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1607
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+80.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2209
_reflns_number_gt                5776
_reflns_number_total             10808
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt53590h2.cif
_cod_data_source_block           6c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7030958--7030964.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C49 H39 B2 Cl3 F2 Fe N8 O6.50 P Pd S'
_cod_database_code               7030963