Synthesis and coordination behavior of Cy(I) bis(phosphaethenyl)pyridine complexes.
Yumiko Nakajima; Yu Shiraishi; Takahiro Tsuchimoto; Fumiyuki Ozawa; Chem.Commun. 47 (2011) 6332–; doi:10.1039/c1cc11315a

data_7106455
_publ_section_title
;
 Synthesis and coordination behavior of Cy(I) bis(phosphaethenyl)pyridine
 complexes.
;
_journal_name_full               Chem.Commun.
_journal_page_first              6332
_journal_paper_doi               10.1039/c1cc11315a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C67.5 H86 Cu F6 N2 P2 Sb'
_chemical_formula_weight         1286.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.242(3)
_cell_angle_beta                 101.392(2)
_cell_angle_gamma                105.3822(15)
_cell_formula_units_Z            2
_cell_length_a                   12.075(3)
_cell_length_b                   17.639(4)
_cell_length_c                   17.853(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     3229.7(13)
_computing_cell_refinement       'Rigaku AFC10/Saturn 70 CCD'
_computing_data_collection       'Rigaku AFC10/Saturn 70 CCD'
_computing_data_reduction        'Rigaku AFC10/Saturn 70 CCD'
_computing_molecular_graphics    'ORTEP3 for windows'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  ' CCD area detector '
_diffrn_measurement_method       ' phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31379
_diffrn_reflns_theta_full        31.59
_diffrn_reflns_theta_max         31.59
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.745
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         17862
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0833
_refine_ls_shift/su_max          6.845
_refine_ls_shift/su_mean         0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+5.9928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                13717
_reflns_number_total             17862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11315a.txt
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C67.50 H86 Cu F6 N2 P2 Sb'
_cod_database_code               7106455