Structural diversity in pyridine and polypyridine adducts of ring slipped manganocene: correlating ligand steric bulk with quantified deviation from ideal hapticity.
Cannella, Anthony F.; Dey, Suman Kr; MacMillan, Samantha N.; Lacy, David C.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 5171–5180; doi:10.1039/C8DT00537K

data_7702185
_publ_section_title
;
 Structural diversity in pyridine and polypyridine adducts of ring slipped
 manganocene: correlating ligand steric bulk with quantified deviation
 from ideal hapticity.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5171
_journal_page_last               5180
_journal_paper_doi               10.1039/C8DT00537K
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H22 Mn N2'
_chemical_formula_sum            'C24 H22 Mn N2'
_chemical_formula_weight         393.37
_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     direct
_audit_creation_date             2018-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-06 deposited with the CCDC.
2018-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.457(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.0321(7)
_cell_length_b                   23.6980(9)
_cell_length_c                   13.6298(5)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.44
_cell_volume                     5727.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      223.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            51305
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.148
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.912
_exptl_crystal_description       Block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         10129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0484P)^2^+0.1831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7525
_reflns_number_total             10129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00537k2.cif
_cod_data_source_block           lac14_a_sq
_cod_database_code               7702185
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C6(H6), C5(H5), C3(H3), C2(H2), C20(H20), C24(H24), C23(H23),
 C22(H22), C21(H21), C17(H17), C16(H16), C15(H15), C19(H19), C18(H18), C33(H33),
  C32(H32), C30(H30), C29(H29), C27(H27), C26(H26), C39(H39), C43(H43),
 C42(H42), C41(H41), C40(H40), C46(H46), C45(H45), C44(H44), C48(H48), C47(H47)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C38(H38A,H38B,H38C), C37(H37A,H37B,
 H37C)
;
_shelx_res_checksum              70233
_shelx_fab_checksum              75157
_olex2_submission_special_instructions 'No special instructions were received'