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_7702178
_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         '3(C20 H18 Mn N2)'
_chemical_formula_sum            'C60 H54 Mn3 N6'
_chemical_formula_weight         1023.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 102.7317(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5006(8)
_cell_length_b                   20.7775(10)
_cell_length_c                   30.9290(13)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.17
_cell_volume                     11596.7(9)
_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 1.000
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            69869
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.252
_diffrn_reflns_theta_min         1.495
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1240 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.9047. 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    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+11.0687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8804
_reflns_number_total             10512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00537k2.cif
_cod_data_source_block           jmc_121602_0m
_cod_database_code               7702178
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C18(H18), C20(H20), C1(H1), C6(H6), C5(H5), C3(H3), C4(H4),
 C13(H13), C19(H19), C17(H17), C12(H12), C7(H7), C2(H2), C9(H9), C14(H14),
 C10(H10), C60(H60), C31(H31), C52(H52), C50(H50), C43(H43), C51(H51), C42(H42),
  C57(H57), C47(H47), C40(H40), C54(H54), C58(H58), C39(H39), C59(H59),
 C53(H53), C44(H44), C45(H45), C24(H24), C22(H22), C25(H25), C37(H37), C46(H46),
  C34(H34), C41(H41), C48(H48), C27(H27), C49(H49), C21(H21), C26(H26),
 C23(H23), C38(H38), C33(H33), C32(H32), C28(H28), C8(H8), C30(H30), C29(H29)
;
_shelx_res_checksum              51391
_shelx_fab_checksum              31022
_olex2_submission_special_instructions ACTA