Probing the factors that influence the conformation of a guanidinato ligand in [(η5-C5Me5)M(NN)X] (NN = chelating N,N′,N′′-tri(o-substituted aryl)guanidinate(1−); X = chloro, azido and triazolato)
Kumar, Robin; Kishan, Ram; Thomas, Jisha Mary; Chinnappan, Sivasankar; Thirupathi, Natesan; New Journal of Chemistry 42 (2018) 1853–; doi:10.1039/C7NJ03766J

data_7056830
_publ_section_title
;
 Probing the factors that influence the conformation of a guanidinato
 ligand in [(\h5-C5Me5)M(NN)X] (NN = chelating
 N,N&#x2032;,N&#x2032;&#x2032;-tri(o-substituted
 aryl)guanidinate(1&#x2212;); X = chloro, azido and triazolato)
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1853
_journal_paper_doi               10.1039/C7NJ03766J
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C29 H28 Cl3 N6 Rh'
_chemical_formula_sum            'C29 H28 Cl3 N6 Rh'
_chemical_formula_weight         669.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2017-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.070(5)
_cell_length_b                   15.118(5)
_cell_length_c                   24.291(5)
_cell_measurement_reflns_used    4432
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.0541
_cell_measurement_theta_min      2.8164
_cell_volume                     2964(2)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    Olex2
_computing_publication_material  'WINGX 2014'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2016 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13534
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.822
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.9417
_exptl_absorpt_correction_T_min  0.7931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2011 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6040
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.0600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5524
_reflns_number_total             6040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03766j2.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7056828--7056838.cif.'
_cod_database_code               7056830
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              13321