Combining photoinduced linkage isomerism and nonlinear optical properties in ruthenium nitrosyl complexes
Mikhailov, Artem; Vuković, Vedran; Kijatkin, Christian; Wenger, Emmanuel; Imlau, Mirco; Woike, Theo; Kostin, Gennadiy; Schaniel, Dominik; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S205252061901357X

data_2108541
_publ_section_title
;
 Combining photoinduced linkage isomerism and nonlinear optical properties
 in ruthenium nitrosyl complexes
;
_journal_coeditor_code           DK5089SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205252061901357X
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'F6 Si, F H12 N5 O Ru'
_chemical_formula_sum            'F7 H12 N5 O Ru Si'
_chemical_formula_weight         360.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_Int_Tables_number      7
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.469(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.7036(4)
_cell_length_b                   7.4260(4)
_cell_length_c                   10.1296(7)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.7580
_cell_measurement_theta_min      2.6590
_cell_volume                     481.00(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4508
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9890
_diffrn_measured_fraction_theta_max 0.8765
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -9.00  95.00   1.00   15.00    --   20.91  57.00 -60.00  104
  2  \w     -9.00  95.00   1.00   15.00    --   20.91  57.00  60.00  104
  3  \w     -9.00  95.00   1.00   15.00    --   20.91  57.00  90.00  104
  4  \w    -53.00  50.00   1.00   15.00    --   20.91 -57.00 150.00  103
  5  \w     -9.00  26.00   1.00   15.00    --   20.91  57.00-180.00   35
  6  \w    -53.00  50.00   1.00   15.00    --   20.91 -57.00 -30.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0933321000
_diffrn_orient_matrix_UB_12      -0.0434867000
_diffrn_orient_matrix_UB_13      0.0019363000
_diffrn_orient_matrix_UB_21      -0.0244839000
_diffrn_orient_matrix_UB_22      0.0748098000
_diffrn_orient_matrix_UB_23      0.0358573000
_diffrn_orient_matrix_UB_31      -0.0547572000
_diffrn_orient_matrix_UB_32      0.0405380000
_diffrn_orient_matrix_UB_33      -0.0639788000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8064
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         32.92
_diffrn_reflns_theta_min         2.74
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.4873
_exptl_crystal_description       block
_exptl_crystal_F_000             349.9500
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.6384
_refine_diff_density_min         -0.6370
_refine_diff_density_rms         0.1043
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_d_res_high            0.6539
_refine_ls_d_res_low             7.4260
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3165
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0232
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+0.2679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.811
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              14
_reflns_limit_l_min              -13
_reflns_number_gt                3066
_reflns_number_total             3165
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            dk5089sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        481.01(5)
_cod_original_sg_symbol_Hall     ' P -2yac '
_cod_database_code               2108541
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2.a Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c), N4(H4a,H4b,H4c), N2(H2a,H2b,H2c), N3(H3a,H3b,H3c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.504
_oxdiff_exptl_absorpt_empirical_full_min 0.729
_cod_database_fobs_code 2108541