Multimetallic Complexes Featuring a Bridging N-heterocyclic Phosphido/Phosphenium Ligand: Synthesis, Structure, and Theoretical Investigation
Baofei Pan; Deirdra A. Evers-McGregor; Mark W. Bezpalko; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 52 (2013) 9583–9589; doi:10.1021/ic4012873

data_4335768
_publ_section_title
;
 Multimetallic Complexes Featuring a Bridging N-heterocyclic
 Phosphido/Phosphenium Ligand: Synthesis, Structure, and Theoretical
 Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9583
_journal_page_last               9589
_journal_paper_doi               10.1021/ic4012873
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C42 H32 Co1 N2 O4 P3 Pt1'
_chemical_formula_sum            'C42 H32 Co N2 O4 P3 Pt'
_chemical_formula_weight         975.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2013-05-22
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 97.472(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4913(12)
_cell_length_b                   18.3892(18)
_cell_length_c                   17.8761(18)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3745.4(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60567
_diffrn_reflns_theta_full        29.522
_diffrn_reflns_theta_max         30.125
_diffrn_reflns_theta_min         1.787
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.348
_exptl_absorpt_correction_T_max  0.21
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.449
_exptl_crystal_size_min          0.354
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.57
_refine_ls_extinction_coef       97(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         10961
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.0060591
_refine_ls_shift/su_mean         0.0000735
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 3.80P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0382
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0382
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10038
_reflns_number_total             10961
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.11
_oxford_diffrn_Wilson_scale      163.28
_oxford_refine_ls_r_factor_ref   0.0192
_oxford_refine_ls_scale          0.079246(6)
_oxford_reflns_number_all        10961
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bfpan_618_0m in P2(1)/c'
_cod_data_source_file            ic4012873_si_002_3.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C42 H32 Co1 N2 O4 P3 Pt1'
_cod_database_code               4335768
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT PT   (    1 ,X'S,U'S)  UNTIL C    (   42 ) 
CONT C    (  340 ,X'S,U[ISO])  UNTIL C    (  381 ) 
CONT EXTPARAM 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   ( 340,X'S) H   (3401,X'S) 
RIDE C   ( 341,X'S) H   (3411,X'S) 
RIDE C   ( 350,X'S) H   (3501,X'S) 
RIDE C   ( 351,X'S) H   (3511,X'S) 
RIDE C   ( 360,X'S) H   (3601,X'S) 
RIDE C   ( 361,X'S) H   (3611,X'S) 
RIDE C   ( 370,X'S) H   (3701,X'S) 
RIDE C   ( 371,X'S) H   (3711,X'S) 
RIDE C   ( 380,X'S) H   (3801,X'S) 
RIDE C   ( 381,X'S) H   (3811,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.397000 , 0.005000 = C(33) TO C(380) 
END                                                                             
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