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_7702183
_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         '0.75(C25 H21 Mn N3), 0.75(C4 H8 O)'
_chemical_formula_sum            'C21.75 H21.75 Mn0.75 N2.25 O0.75'
_chemical_formula_weight         367.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                94.364(4)
_cell_angle_beta                 91.606(4)
_cell_angle_gamma                115.268(3)
_cell_formula_units_Z            8
_cell_length_a                   14.905(2)
_cell_length_b                   16.420(3)
_cell_length_c                   16.608(3)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.82
_cell_measurement_theta_min      2.45
_cell_volume                     3656.8(11)
_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_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50450
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.140
_diffrn_reflns_theta_min         1.514
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1396 before and 0.0454 after correction. The Ratio of minimum to maximum transmission is 0.8232. The \l/2 correction factor is Not present.'
_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    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         23321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0507P)^2^+2.4868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16541
_reflns_number_total             23321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00537k2.cif
_cod_data_source_block           dcl-005-skd-086
_cod_original_cell_volume        3656.7(10)
_cod_database_code               7702183
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C86(H86A,H86B), C84(H84A,H84B), C76(H76A,H76B), C77(H77A,
 H77B), C78(H78A,H78B), C79(H79A,H79B), C82(H82A,H82B), C83(H83A,H83B),
 C81(H81A,H81B), C80(H80A,H80B), C0AA(H0AA,H0AB)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C50(H50), C48(H48), C47(H47), C27(H27), C44(H44), C32(H32),
 C26(H26), C42(H42), C39(H39), C36(H36), C43(H43), C28(H28), C49(H49), C38(H38),
  C31(H31), C35(H35), C30(H30), C29(H29), C33(H33), C34(H34), C69(H69),
 C57(H57), C68(H68), C67(H67), C51(H51), C56(H56), C55(H55), C64(H64), C54(H54),
  C58(H58), C61(H61), C52(H52), C63(H63), C53(H53), C72(H72), C75(H75),
 C59(H59), C62(H62), C74(H74), C60(H60), C73(H73), C14(H14), C13(H13), C17(H17),
  C19(H19), C22(H22), C12(H12), C25(H25), C11(H11), C24(H24), C23(H23), C3(H3),
 C2(H2), C1(H1), C5(H5), C18(H18), C4(H4), C9(H9), C10(H10), C8(H8), C6(H6),
 C7(H7)
;
_shelx_res_checksum              84437
_olex2_submission_special_instructions 'No special instructions were received'