Stepwise Deoxygenation of Nitrite as a Route to Two Families of Ruthenium Corroles: Group 8 Periodic Trends and Relativistic Effects.
Alemayehu, Abraham B.; Vazquez-Lima, Hugo; Gagnon, Kevin J.; Ghosh, Abhik; Inorganic chemistry 56 (2017) 5285–5294; doi:10.1021/acs.inorgchem.7b00377

data_4349426
_publ_section_title
;
 Stepwise Deoxygenation of Nitrite as a Route to Two Families of Ruthenium
 Corroles: Group 8 Periodic Trends and Relativistic Effects.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5285
_journal_page_last               5294
_journal_paper_doi               10.1021/acs.inorgchem.7b00377
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C37 H23 N5 Ru'
_chemical_formula_weight         638.67
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
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_cell_angle_alpha                90
_cell_angle_beta                 100.249(2)
_cell_angle_gamma                90
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_cell_length_a                   12.1216(5)
_cell_length_b                   22.0370(9)
_cell_length_c                   10.7799(5)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.009
_cell_measurement_theta_min      2.744
_cell_volume                     2833.6(2)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         36.042
_diffrn_reflns_theta_min         2.117
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS, Madison WI'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       blade
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         10358
_refine_ls_number_restraints     343
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+3.5334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7564
_reflns_number_total             10358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00377_si_002.cif
_cod_data_source_block           RuNTPC
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349426
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              7103
_shelx_hkl_checksum              66793
_shelx_fab_checksum              13142