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_4124586
_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_formula_moiety         'C32 H93 Ca1 N16 O5 P5, C8 Fe2 O8'
_chemical_formula_sum            'C40 H93 Ca Fe2 N16 O13 P5'
_chemical_formula_weight         1312.93
_chemical_name_systematic
;
[Ca(HMPA)5(MeCN)][Fe2CO8]
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.2009(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2558(3)
_cell_length_b                   21.4450(3)
_cell_length_c                   43.1110(7)
_cell_measurement_reflns_used    20346
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      3
_cell_volume                     13010.1(4)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            76780
_diffrn_reflns_theta_full        74.450
_diffrn_reflns_theta_max         76.752
_diffrn_reflns_theta_min         3.140
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.969
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.22
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1450
_refine_ls_number_reflns         17162
_refine_ls_number_restraints     268
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0934
_refine_ls_shift/su_max          0.0044989
_refine_ls_shift/su_mean         0.0000664
_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: 
 16.3 0.213 8.02 4.12 -4.26 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1084
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0899
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              54
_reflns_limit_l_min              0
_reflns_number_gt                19569
_reflns_number_total             27024
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.84
_oxford_diffrn_Wilson_scale      0.90
_oxford_refine_ls_r_factor_ref   0.0846
_oxford_refine_ls_scale          1.0237(17)
_oxford_reflns_number_all        26921
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja5b07866_si_002.cif
_cod_data_source_block           compound_S5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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 '
_cod_original_formula_sum        'C40 H93 Ca1 Fe2 N16 O13 P5'
_cod_database_code               4124586