A series of C3-symmetric heterobimetallic Cr–M (M = Fe, Co and Cu) complexes
Kuppuswamy, Subramaniam; Bezpalko, Mark W.; Powers, Tamara M.; Wilding, Matthew J. T.; Brozek, Carl K.; Foxman, Bruce M.; Thomas, Christine M.; Chemical Science 5 (2014) 1617–; doi:10.1039/c3sc52943f

data_1513869
_publ_section_title
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 A series of C3-symmetric heterobimetallic Cr--M (M = Fe, Co and Cu)
 complexes
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_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1617
_journal_paper_doi               10.1039/c3sc52943f
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C48 H60 Co1 Cr1 N3 P4'
_chemical_formula_sum            'C48 H60 Co Cr N3 P4'
_chemical_formula_weight         913.85
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2013-04-05
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   16.2999(6)
_cell_length_b                   16.2999(6)
_cell_length_c                   22.8438(9)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     5256.2(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.052
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5119
_diffrn_reflns_theta_full        30.023
_diffrn_reflns_theta_max         30.023
_diffrn_reflns_theta_min         1.783
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.220
_platon_squeeze_details
;
During the structure solution, electron density difference 
maps revealed that there were considerable disordered 
solvent molecules which could not be successfully modeled.  
From history, the remaining solvate was likely diethyl ether 
in a volume of 923.6 \%A3 per unit cell (17.6%).  It 
appeared that the cavity area contained ca. three ether 
molecules, located near the  position at (0, 0, 0). 
Modeling with or without restraints was unsuccessful, 
as was step by step acquisition of peaks using successive 
electron density difference maps.  Thus, the structure 
factors were modified using the PLATON SQUEEZE technique, 
in order to produce a "solvate-free" structure factor set.  
PLATON reported a total electron density of 97 e- per unit 
cell, likely representing three diethyl ether molecules, 
consistent with our earlier observations.  Use of the 
SQUEEZE technique resulted in a decrease of ca. 1.9 % in R.   
;
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.71
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0465
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         5119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.0018760
_refine_ls_shift/su_mean         0.0000844
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.59P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0968
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0968
_reflns_limit_h_max              0
_reflns_limit_h_min              -19
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                4031
_reflns_number_total             5119
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.32
_oxford_diffrn_Wilson_scale      162.43
_oxford_refine_ls_r_factor_ref   0.0431
_oxford_refine_ls_scale          0.078657(18)
_oxford_reflns_number_all        5119
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'sk_870_0m in P-3c1'
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) H   (  23,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) H   (  33,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,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) H   ( 162,X'S) H   ( 163,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c3sc52943f.txt
_cod_data_source_block           5
_cod_original_sg_symbol_Hall     '-P 3 2"c '
_cod_original_sg_symbol_H-M      'P -3 c 1 '
_cod_original_formula_sum        'C48 H60 Co1 Cr1 N3 P4'
_cod_database_code               1513869