Isolation of Au-, Co-η1PCO and Cu-η2PCO complexes, conversion of an Ir‒η1PCO complex into a dimetalladiphosphene, and an interaction-free PCO anion
Liu, Liu; Ruiz, David A.; Dahcheh, Fatme; Bertrand, Guy; Suter, Riccardo; Tondreau, Aaron M.; Grützmacher, Hansjörg; Chem. Sci. 7 (2016) 2335–; doi:10.1039/C5SC04504E

data_1541889
_publ_section_title
;
 Isolation of Au-, Co-\h1PCO and Cu-\h2PCO complexes, conversion of an
 Ir--\h1PCO complex into a dimetalladiphosphene, and an interaction-free
 PCO anion
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              2335
_journal_paper_doi               10.1039/C5SC04504E
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C49 H79 Cu N5 O P'
_chemical_formula_weight         848.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-05-31 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.409(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6627(14)
_cell_length_b                   16.2794(15)
_cell_length_c                   23.264(3)
_cell_measurement_reflns_used    9143
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.50
_cell_volume                     4744.1(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.1293
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20548
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         8282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+2.6742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                4839
_reflns_number_total             8282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04504e2.cif
_cod_data_source_block           compound6
_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1541885--1541894.cif.

2017-03-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C98 H158 Cu2 N10 O2 P2'
_cod_original_formula_weight         1697.36
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1541889