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_4342897
_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 H101 Fe N4 Na, C5 H12'
_chemical_formula_sum            'C105 H113 Fe N4 Na'
_chemical_formula_weight         1509.83
_chemical_name_common            Na[HFe(CNArMes2)4]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 90.479(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4873(10)
_cell_length_b                   27.8985(17)
_cell_length_c                   22.7298(14)
_cell_measurement_reflns_used    2811
_cell_measurement_temperature    100
_cell_measurement_theta_max      56.388
_cell_measurement_theta_min      2.507
_cell_volume                     8552.4(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (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 0.923
_diffrn_measured_fraction_theta_max 0.923
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_laue_measured_fraction_full 0.923
_diffrn_reflns_laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17277
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        57.708
_diffrn_reflns_theta_max         57.708
_diffrn_reflns_theta_min         2.507
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.840
_exptl_absorpt_correction_T_max  0.150099
_exptl_absorpt_correction_T_min  0.066878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0601 before and 0.0378 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0736 before and 0.0385 after correction.
 The Ratio of minimum to maximum transmission is 0.44.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 47890 reflections, Rint = 0.0865
 (14760 with I > 3sig(I), Rint = 0.0419)
;
_exptl_crystal_colour            Red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         10905
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7134
_reflns_number_total             10905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00730_si_002.cif
_cod_data_source_block           JFigCu108
_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_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               4342897
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.909
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4S-C5S = C5SB-C4SB = C4S-C3S = C2S-C3S = C2SB-C3SB = C1S-C2S = C2SB-C1SB
 1.54 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C5S) = Uanis(C5SB)
Uanis(C4S) = Uanis(C4SB)
Uanis(C3S) = Uanis(C3SB)
Uanis(C2S) = Uanis(C2SB)
Uanis(C1SB) = Uanis(C1S)
4. Rigid body (RIGU) restrains
 C1S, C1SB, C2S, C2SB, C3S, C3SB, C4S, C4SB, C5S, C5SB
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C1SB)=Sof(H1SD)=Sof(H1SE)=Sof(H1SF)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=
 Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=Sof(C4SB)=Sof(H4SC)=Sof(H4SD)=Sof(C5SB)=
 Sof(H5SD)=Sof(H5SE)=Sof(H5SF)=1-FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=
 Sof(H5SC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C2SB(H2SC,H2SD), C3S(H3SA,H3SB), C3SB(H3SC,H3SD), C4S(H4SA,
 H4SB), C4SB(H4SC,H4SD)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C13(H13), C15(H15), C22(H22), C24(H24), C31(H31),
 C32(H32), C33(H33), C37(H37), C39(H39), C46(H46), C48(H48), C55(H55), C56(H56),
  C57(H57), C61(H61), C63(H63), C70(H70), C72(H72), C79(H79), C80(H80),
 C81(H81), C85(H85), C87(H87), C94(H94), C96(H96)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C89(H89A,
 H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C98(H98A,H98B,H98C),
 C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C1S(H1SA,H1SB,H1SC), C1SB(H1SD,H1SE,
 H1SF), C5S(H5SA,H5SB,H5SC), C5SB(H5SD,H5SE,H5SF)
;
_shelx_res_checksum              92439
_shelx_hkl_checksum              46856
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'