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_4342894
_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         'C53 H50 Fe N2 O3'
_chemical_formula_sum            'C53 H50 Fe N2 O3'
_chemical_formula_weight         818.80
_chemical_name_common            Fe(CO)3(CNArMes2)2
_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             2015-03-05
_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                 117.941(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.7165(11)
_cell_length_b                   13.6599(5)
_cell_length_c                   27.7314(11)
_cell_measurement_reflns_used    2929
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.566
_cell_measurement_theta_min      2.660
_cell_volume                     8940.7(7)
_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    'ShelXT (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 0.981
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1127
_diffrn_reflns_laue_measured_fraction_full 0.981
_diffrn_reflns_laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26325
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         2.095
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6148
_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 0.1059 before and 0.0365 after correction.
 The Ratio of minimum to maximum transmission is 0.60.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1649 before and 0.0408 after correction.
 The Ratio of minimum to maximum transmission is 0.60.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 50707 reflections, Rint = 0.0558
 (11651 with I > 3sig(I), Rint = 0.0373)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         26325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0396P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16717
_reflns_number_total             26325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00730_si_002.cif
_cod_data_source_block           JFig951
_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 'Yellow' changed to 'yellow'
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_original_cell_volume        8940.7(6)
_cod_database_code               4342894
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.954
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8289(6) 0.1711(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C14(H14), C16(H16), C23(H23), C25(H25), C32(H32),
 C33(H33), C34(H34), C38(H38), C40(H40), C47(H47), C49(H49), C8'(H8'), C9'(H9'),
  C10'(H10'), C14'(H14'), C16'(H16'), C23'(H23'), C25'(H25'), C32'(H32'),
 C33'(H33'), C38'(H38'), C40'(H40'), C47'(H47'), C49'(H49')
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C18'(H18D,H18E,H18F), C19'(H19D,H19E,H19F), C20'(H20D,
 H20E,H20F), C27'(H27D,H27E,H27F), C28'(H28D,H28E,H28F), C29'(H29D,H29E,H29F),
 C42'(H42D,H42E,H42F), C43'(H43D,H43E,H43F), C44'(H44D,H44E,H44F), C51'(H51D,
 H51E,H51F), C52'(H52D,H52E,H52F), C53'(H53D,H53E,H53F)
;
_shelx_res_checksum              34522
_shelx_hkl_checksum              31232
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'