Synthesis, structures, and reactivity of isomers of [RuCp*(1,4-(Me<sub>2</sub>N)<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)]<sub>2</sub>.
Longhi, Elena; Risko, Chad; Bacsa, John; Khrustalev, Victor; Rigin, Sergei; Moudgil, Karttikay; Timofeeva, Tatiana V.; Marder, Seth R.; Barlow, Stephen; Dalton transactions (Cambridge, England : 2003) 50 (2021) 13020–13030; doi:10.1039/d1dt02155a

data_7708133
_publ_section_title
;
 Synthesis, structures, and reactivity of isomers of
 [RuCp*(1,4-(Me<sub>2</sub>N)<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)]<sub>2</sub>.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13020
_journal_page_last               13030
_journal_paper_doi               10.1039/d1dt02155a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H62 N4 Ru2'
_chemical_formula_sum            'C40 H62 N4 Ru2'
_chemical_formula_weight         801.095
_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_Int_Tables_number      14
_audit_creation_date             2021-05-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-14 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.410(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2872(4)
_cell_length_b                   8.62433(19)
_cell_length_c                   15.3075(4)
_cell_measurement_reflns_used    12853
_cell_measurement_temperature    105(8)
_cell_measurement_theta_max      37.8250
_cell_measurement_theta_min      2.7120
_cell_volume                     1818.34(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.3-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9863
_diffrn_measured_fraction_theta_max 0.9892
_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    -41.00  41.00   0.50    5.00    --   27.43 -36.00 -33.00  164
  2  \w    -23.00   2.00   0.50    5.00    --  -27.43  36.00 122.00   50
  3  \w     16.00 102.00   0.50    5.00    --   27.43  36.00 122.00  172
  4  \w      9.00  98.00   0.50   16.00    --   27.43  57.00 150.00  178
  5  \w     42.00  68.00   0.50   16.00    --   27.43 178.00 120.00   52
  6  \w     43.00 101.00   0.50   16.00    --   27.43 178.00 -30.00  116
  7  \w     47.00  98.00   0.50   16.00    --   27.43 178.00 -90.00  102
  8  \w    -72.00 -47.00   0.50   16.00    --  -27.43 -36.00 -33.00   50
  9  \w    -91.00 -64.00   0.50   16.00    --  -27.43 178.00 120.00   54
 10  \w   -101.00 -75.00   0.50   16.00    --  -27.43 178.00  90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0209670000
_diffrn_orient_matrix_UB_12      0.0266148000
_diffrn_orient_matrix_UB_13      0.0447956000
_diffrn_orient_matrix_UB_21      -0.0460970000
_diffrn_orient_matrix_UB_22      0.0265829000
_diffrn_orient_matrix_UB_23      0.0027261000
_diffrn_orient_matrix_UB_31      -0.0091424000
_diffrn_orient_matrix_UB_32      -0.0731456000
_diffrn_orient_matrix_UB_33      0.0172653000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_Laue_measured_fraction_full 0.9863
_diffrn_reflns_Laue_measured_fraction_max 0.9892
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18861
_diffrn_reflns_point_group_measured_fraction_full 0.9863
_diffrn_reflns_point_group_measured_fraction_max 0.9892
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.74
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.463
_exptl_crystal_description       plate
_exptl_crystal_F_000             831.270
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.3744
_refine_diff_density_min         -1.1866
_refine_diff_density_rms         0.1486
_refine_ls_d_res_high            0.7702
_refine_ls_d_res_low             7.4460
_refine_ls_extinction_coef       0.0035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     244
_refine_ls_number_reflns         18861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0021
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0059
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+3.8871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -17
_reflns_limit_k_max              10
_reflns_limit_k_min              -11
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                14694
_reflns_number_total             18861
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt02155a2.cif
_cod_data_source_block           EL-II-41
_cod_depositor_comments
'Adding full bibliography for 7708131--7708134.cif.'
_cod_original_cell_volume        1818.35(8)
_cod_database_code               7708133
_chemical_oxdiff_formula         'C80  H124  N8  Ru4  '
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9339(7)
 0.0661(7)
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 Ternary CH refined with riding coordinates:
 C9(H9), C10(H10), C5(H5), C4(H4)
3.b Idealised Me refined with riding coordinates and stretchable bonds:
 C18(H18a,H18b,H18c), C17(H17a,H17b,H17c)
3.c Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C7(H7a,H7b,H7c), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c),
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C8(H8a,H8b,H8c)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 1.592
_oxdiff_exptl_absorpt_empirical_full_min 0.735