Preparation of a novel diphosphine-palladium macrocyclic complex possessing a molecular recognition site. Oxidative addition studies.
Larsen, Jens; Rasmussen, Brian S; Hazell, Rita G; Skrydstrup, Troels; Chemical communications (Cambridge, England)  (2004) 202–203; doi:10.1039/b309863j

data_7102411
_publ_section_title
;
 Preparation of a novel diphosphine-palladium macrocyclic complex
 possessing a molecular recognition site. Oxidative addition studies.
;
_journal_issue                   2
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              202
_journal_page_last               203
_journal_paper_doi               10.1039/b309863j
_journal_year                    2004
_chemical_formula_moiety
'C64 H51 I N6 O4 P2 Pd, C9 H12 N2 O3, 2(C H Cl3)'
_chemical_formula_sum            'C75 H65 Cl6 I N8 O7 P2 Pd'
_chemical_formula_weight         1698.41
_chemical_name_common            'Pd-I-benzene-macrocycle, loose barbiturate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.000
_cell_angle_beta                 91.177(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   9.743(2)
_cell_length_b                   21.892(3)
_cell_length_c                   17.360(3)
_cell_measurement_reflns_used    5465
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      1.9
_cell_volume                     3702(1)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;
ORTEP-III (Burnett & Johnson,  1996), KRYSTAL
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;
SIR97 (Altomare et al., 1997 ), KRYSTAL
;
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.097
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35623
_diffrn_reflns_reduction_process 35623
_diffrn_reflns_theta_full        26.4
_diffrn_reflns_theta_max         28.4
_diffrn_reflns_theta_min         1.9
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.3(1)
_refine_diff_density_min         -3.0(1)
_refine_ls_abs_structure_details
; A parameter according to Rogers (1981) was refined using the full dataset
(averaged to allow determination of the absolute structure) of 11089
significant reflexions, including 4710 Bijvoet pairs. The parameter
refined to close to 0 in agreement with the fact that the structure
deviates only slightly from space group P 21/m, and with the fact that
the deviations are found far from the heavy atoms. Twinning is likely to
occur in this sort of structure.
;
_refine_ls_abs_structure_Rogers  0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.376
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     898
_refine_ls_number_reflns         11089
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.0019
_refine_ls_shift/su_mean         0.00005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
w= 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^- |F|}^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.044
_reflns_number_gt                11089
_reflns_number_total             16807
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            b309863j.txt
_cod_data_source_block           cpd_7
_cod_depositor_comments
;
 Adding the '_geom_hbond_atom_site_label_A' data item. Values of the
 data item were determined from the geometry of the molecule.

 Antanas Vaitkus,
 2017-03-06

The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 98 times.

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

The following automatic conversions were performed:
data name '_geom_bond_atom_site_label_D' replaced with
'_geom_hbond_atom_site_label_D' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_atom_site_label_H' replaced with
'_geom_hbond_atom_site_label_H' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_distance_DH' replaced with '_geom_hbond_distance_DH'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_HA' replaced with
'_geom_hbond_distance_HA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_DA' replaced with
'_geom_hbond_distance_DA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_angle_DHA' replaced with '_geom_hbond_angle_DHA' as
specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7102411