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_7702180
_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         'C22 H18 Mn N2'
_chemical_formula_sum            'C22 H18 Mn N2'
_chemical_formula_weight         365.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-06
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.0154(6)
_cell_length_b                   26.5037(15)
_cell_length_c                   11.5756(7)
_cell_measurement_reflns_used    7404
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.40
_cell_volume                     3379.5(3)
_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      90
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0772
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            45577
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.443
_diffrn_reflns_theta_min         1.537
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1739 before and 0.0711 after correction. The Ratio of minimum to maximum transmission is 0.8444. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6871
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0594P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5812
_reflns_number_total             6871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00537k2.cif
_cod_data_source_block           dcl_001_skd_056
_cod_database_code               7702180
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.85(2)
 0.15(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C18(H18), C20(H20), C16(H16), C1(H1), C6(H6), C4(H4),
 C13(H13), C15(H15), C12(H12), C3(H3), C7(H7), C10(H10), C5(H5), C31(H31),
 C41(H41), C27(H27), C33(H33), C42(H42), C24(H24), C34(H34), C35(H35), C30(H30),
  C32(H32), C40(H40), C38(H38), C29(H29), C2(H2), C19(H19), C11(H11), C26(H26),
 C25(H25), C37(H37), C23(H23), C28(H28)
;
_shelx_res_checksum              26547
_olex2_submission_original_sample_id SKD-01-56
_olex2_submission_special_instructions 'No special instructions were received'