Synthesis and Structure of Chromium(VI) Nitrido Cyclopentadienyl Complexes
Billow, Brennan S.; Bemowski, Ross D.; DiFranco, Stephen A.; Staples, Richard J.; Odom, Aaron L.; Organometallics 34 (2015) 4567–; doi:10.1021/acs.organomet.5b00661

data_4086302
_publ_section_title
;
 Synthesis and Structure of Chromium(VI) Nitrido Cyclopentadienyl
 Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4567
_journal_paper_doi               10.1021/acs.organomet.5b00661
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C12 H10 Fe O2'
_chemical_formula_sum            'C12 H10 Fe O2'
_chemical_formula_weight         242.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     direct
_audit_creation_date             2015-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.154(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5220(16)
_cell_length_b                   7.4596(9)
_cell_length_c                   11.2323(14)
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.19
_cell_volume                     1038.6(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8231
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.391
_diffrn_reflns_theta_min         3.187
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0602 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8484. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0319P)^2^+0.3677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1534
_reflns_number_total             1900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00661_si_002.cif
_cod_data_source_block           fecpco173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_database_code               4086302
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.033) H3(0.039) H4(0.044) H5(0.039) H6(0.043) H7(0.037)
 H8(0.04) H9(0.046) H10(0.047)
 Fixed X: H2(0.8155) H3(0.9949) H4(0.9817) H5(0.7934) H6(0.813001) H7(0.9042)
 H8(0.7927) H9(0.6324) H10(0.6441)
 Fixed Y: H2(0.609) H3(0.653201) H4(0.8777) H5(0.972799) H6(0.9615) H7(1.0399)
 H8(1.276499) H9(1.348201) H10(1.153301)
 Fixed Z: H2(0.9598) H3(0.902699) H4(0.73) H5(0.6795) H6(1.1497) H7(0.9697)
 H8(0.8491) H9(0.9561) H10(1.1407)
;
_shelx_res_checksum              10387
_shelx_hkl_checksum              772
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'mounted on nylon loop with paratone oil'
_olex2_submission_original_sample_id 'Fe(CP)2(CO)2 173 10s'
_olex2_submission_special_instructions 'No special instructions were received'