Surface functionalization of dinuclear clathrochelates via Pd-catalyzed cross-coupling reactions: facile synthesis of polypyridyl metalloligands.
Marmier, Mathieu; Cecot, Giacomo; Curchod, Basile F. E.; Pattison, Philip; Solari, Euro; Scopelliti, Rosario; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8422–8427; doi:10.1039/c6dt01288d

data_7039112
_publ_section_title
;
 Surface functionalization of dinuclear clathrochelates via Pd-catalyzed
 cross-coupling reactions: facile synthesis of polypyridyl metalloligands.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8422
_journal_page_last               8427
_journal_paper_doi               10.1039/c6dt01288d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C49 H32 B2 N11 O9 Zn2, C8 H20 N'
_chemical_formula_sum            'C57 H52 B2 N12 O9 Zn2'
_chemical_formula_weight         1201.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-02
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_audit_update_record
;
2016-02-15 deposited with the CCDC.
2016-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9652(2)
_cell_length_b                   25.8649(2)
_cell_length_c                   14.10590(10)
_cell_measurement_reflns_used    10973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.8550
_cell_measurement_theta_min      1.9910
_cell_volume                     6189.71(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69791
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46615
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        24.755
_diffrn_reflns_theta_max         26.822
_diffrn_reflns_theta_min         1.546
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'R. H. Blessing, Acta Cryst. A, 1995, 51, 33-38'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 2953 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.051(4)
_refine_ls_extinction_coef       0.0041(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0543P)^2^+3.1273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                6698
_reflns_number_total             6700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01288d2.cif
_cod_data_source_block           mm637j1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
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.

'_atom_sites_solution_secondary' value 'Difmap' changed to 'difmap'
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 7039111--7039113.cif.
;
_cod_database_code               7039112
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.691
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C012(H01A,H01B), C017(H01F,H01G)
2.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00I(H00I), C00K(H00K), C00M(H00M), C00N(H00N),
 C00O(H00O), C00R(H00R), C00U(H00U), C00V(H00V), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C011(H011), C013(H013), C016(H016)
2.c Idealised Me refined as rotating group:
 C014(H01C,H01D,H01E), C019(H01H,H01I,H01J)
;
_shelx_res_checksum              74046
_shelx_fab_checksum              4382
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'