Toward Permetalated Alkyne/Azide 3 + 2 or “Click” Cycloadducts
Clough, Melissa C.; Zeits, Paul D.; Bhuvanesh, Nattamai; Gladysz, John A.; Organometallics 31 (2012) 5231–; doi:10.1021/om300542a

data_4078934
_publ_section_title
;
 Toward Permetalated Alkyne/Azide 3 + 2 or &#x201C;Click&#x201D;
 Cycloadducts
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_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5231
_journal_paper_doi               10.1021/om300542a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C66 H51 Br Cl4 F5 N3 O7 P2 Pt Re2'
_chemical_formula_weight         1944.24
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1623(16)
_cell_length_b                   46.074(6)
_cell_length_c                   11.9613(16)
_cell_measurement_reflns_used    9475
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.43
_cell_volume                     6702.7(15)
_computing_cell_refinement
; 
  APEX-II(BRUKER-NONIUS, 2003) 
;
_computing_data_collection       'APEX-II (BRUKER-NONIUS, 2003)'
_computing_data_reduction        APEX-II
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       'omega 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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            134479
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.557
_exptl_absorpt_correction_T_max  0.6568
_exptl_absorpt_correction_T_min  0.1381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.949
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.276
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         15360
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0264
_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 
 [1.00000+-1.00000exp(-15.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+10.4159*P+(0.0360P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                14832
_reflns_number_total             15360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300542a_si_002.cif
_cod_data_source_block           p21212
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_database_code               4078934