Synthesis and protonation of an encumbered iron tetraisocyanide dianion.
Mokhtarzadeh, Charles C.; Margulieux, Grant W.; Carpenter, Alex E.; Weidemann, Nils; Moore, Curtis E.; Rheingold, Arnold L.; Figueroa, Joshua S.; Inorganic chemistry 54 (2015) 5579–5587; doi:10.1021/acs.inorgchem.5b00730

data_4342892
_publ_section_title
;
 Synthesis and protonation of an encumbered iron tetraisocyanide dianion.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5579
_journal_page_last               5587
_journal_paper_doi               10.1021/acs.inorgchem.5b00730
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C100 H100 Fe N4 Na2'
_chemical_formula_sum            'C100 H100 Fe N4 Na2'
_chemical_formula_weight         1459.66
_chemical_name_common            Na2[Fe(CNArMes2)4]
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.721(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1109(10)
_cell_length_b                   11.8497(4)
_cell_length_c                   27.5348(10)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.927
_cell_measurement_theta_min      4.135
_cell_volume                     7969.3(5)
_computing_cell_refinement       'SAINT v8.18C (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.18C (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_laue_measured_fraction_full 0.957
_diffrn_reflns_laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            53195
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         69.669
_diffrn_reflns_theta_min         3.730
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  0.3216
_exptl_absorpt_correction_T_min  0.1907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.5930.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       Block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         14070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+9.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11340
_reflns_number_total             14070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00730_si_002.cif
_cod_data_source_block           JFigCu100
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_modifier' value 'Dark' changed to 'dark'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_primary' value 'Red' changed to 'red'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 

 Adding full bibliography for 4342892--4342900.cif.
;
_cod_database_code               4342892
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.492
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C11(H11), C13(H13), C20(H20), C22(H22), C29(H29),
 C30(H30), C31(H31), C35(H35), C37(H37), C44(H44), C46(H46), C5'(H5'), C6'(H6'),
  C7'(H7'), C11'(H11'), C13'(H13'), C20'(H20'), C22'(H22'), C29'(H29'),
 C30'(H30'), C31'(H31'), C35'(H35'), C37'(H37'), C44'(H44'), C46'(H46')
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C15'(H15D,H15E,H15F), C16'(H16D,H16E,H16F), C17'(H17D,
 H17E,H17F), C24'(H24D,H24E,H24F), C25'(H25D,H25E,H25F), C26'(H26D,H26E,H26F),
 C39'(H39D,H39E,H39F), C40'(H40D,H40E,H40F), C41'(H41D,H41E,H41F), C48'(H48D,
 H48E,H48F), C49'(H49D,H49E,H49F), C50'(H50D,H50E,H50F)
;
_shelx_res_checksum              18447
_shelx_hkl_checksum              32530
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'