Probing the Limits of Alkaline Earth-Transition Metal Bonding: An Experimental and Computational Study.
Blake, Matthew P.; Kaltsoyannis, Nikolas; Mountford, Philip; Journal of the American Chemical Society 137 (2015) 12352–12368; doi:10.1021/jacs.5b07866

data_4124584
_publ_section_title
;
 Probing the Limits of Alkaline Earth-Transition Metal Bonding: An
 Experimental and Computational Study.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12352
_journal_page_last               12368
_journal_paper_doi               10.1021/jacs.5b07866
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H15 Ca1 Fe2 N5 O8'
_chemical_formula_sum            'C18 H15 Ca Fe2 N5 O8'
_chemical_formula_weight         581.12
_chemical_name_systematic
;
Ca{Fe2(CO)8}(MeCN)5
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n 2a'
_symmetry_space_group_name_H-M   'P 21 c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0633(3)
_cell_length_b                   16.3836(3)
_cell_length_c                   19.0298(4)
_cell_measurement_reflns_used    11512
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     5008.16(17)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20833
_diffrn_reflns_theta_full        26.954
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         5.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.70
_refine_diff_density_min         -0.72
_refine_ls_abs_structure_details 'Flack (1983), 4944 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.548(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         8619
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.0014740
_refine_ls_shift/su_mean         0.0000313
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 -0.208 -1.67 -0.624 -0.691 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0310
_refine_ls_wR_factor_gt          0.0273
_refine_ls_wR_factor_ref         0.0262
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                9320
_reflns_number_total             10853
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0477
_oxford_refine_ls_scale          0.17645(15)
_oxford_reflns_number_all        10853
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja5b07866_si_002.cif
_cod_data_source_block           compound_S3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/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 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21 c n '
_cod_original_formula_sum        'C18 H15 Ca1 Fe2 N5 O8'
_cod_database_code               4124584