A regioselectively 1,1′,3,3′-tetrazincated ferrocene complex displaying core and peripheral reactivity
Honeyman, Gordon W.; Armstrong, David R.; Clegg, William; Hevia, Eva; Kennedy, Alan R.; McLellan, Ross; Orr, Samantha A.; Parkinson, John A.; Ramsay, Donna L.; Robertson, Stuart D.; Towie, Stephen; Mulvey, Robert E.; Chemical Science 11 (2020) 6510–6520; doi:10.1039/D0SC01612H

data_1557680
_publ_section_title
;
 A regioselectively 1,1&#x2032;,3,3&#x2032;-tetrazincated ferrocene
 complex displaying core and peripheral reactivity
;
_journal_issue                   25
_journal_name_full               'Chemical Science'
_journal_page_first              6510
_journal_page_last               6520
_journal_paper_doi               10.1039/D0SC01612H
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C39 H42 N7 Na Zn'
_chemical_formula_sum            'C39 H42 N7 Na Zn'
_chemical_formula_weight         697.15
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-12-17 deposited with the CCDC.	2020-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8556(2)
_cell_length_b                   17.4144(4)
_cell_length_c                   23.9796(5)
_cell_measurement_reflns_used    3475
_cell_measurement_temperature    123.05(10)
_cell_measurement_theta_max      70.6260
_cell_measurement_theta_min      5.0160
_cell_volume                     3698.01(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0268
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega   -4.00   42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 46

  2 omega   -4.00   42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -30.0000 46

  3 omega   30.00  128.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   37.0000  150.0000 98

  4 omega   26.00  126.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000 -150.0000 100

  5 omega   40.00   92.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000 -120.0000 52

  6 omega   39.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -180.0000 55

  7 omega   42.00  105.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000    0.0000 63

  8 omega   42.00  105.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -60.0000 63

  9 omega   42.00  142.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -150.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0244554000
_diffrn_orient_matrix_UB_12      0.0374639000
_diffrn_orient_matrix_UB_13      0.0575018000
_diffrn_orient_matrix_UB_21      -0.1574754000
_diffrn_orient_matrix_UB_22      0.0275520000
_diffrn_orient_matrix_UB_23      -0.0185363000
_diffrn_orient_matrix_UB_31      -0.0696266000
_diffrn_orient_matrix_UB_32      -0.0752808000
_diffrn_orient_matrix_UB_33      0.0218099000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9912
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.159
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0433P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                4534
_reflns_number_total             6328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01612h2.cif
_cod_data_source_block           RMSO19b
_cod_depositor_comments
;Adding full bibliography for 1557679--1557682.cif.

 Adding full bibliography for 1557679--1557682.cif.
;
_cod_database_code               1557680
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 97.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48543 0.51457
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35)
3.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              27935
_olex2_submission_original_sample_id RMSO19b
_olex2_submission_special_instructions 'No special instructions were received'