Role of torsional strain in the ring-opening polymerisation of low strain [n]nickelocenophanes
Musgrave, Rebecca A.; Hailes, Rebekah L. N.; Annibale, Vincent T.; Manners, Ian; Chemical Science  (2019) –; doi:10.1039/C9SC02624J

data_1552313
_publ_section_title
;
 Role of torsional strain in the ring-opening polymerisation of low strain
 [n]nickelocenophanes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02624J
_journal_year                    2019
_chemical_formula_moiety         'C14 H16 Ni'
_chemical_formula_sum            'C14 H16 Ni'
_chemical_formula_weight         242.98
_chemical_name_systematic        1-Methyltricarba[3]nickelocenophane
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-28 deposited with the CCDC.    2019-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.465(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9016(6)
_cell_length_b                   9.6856(7)
_cell_length_c                   14.8574(11)
_cell_measurement_reflns_used    3117
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.53
_cell_volume                     1114.37(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13870
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.026
_diffrn_reflns_theta_min         2.526
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.702
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0639 before and 0.0513 after correction. The Ratio of minimum to maximum transmission is 0.8466. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2697
_refine_ls_number_restraints     808
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+0.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2092
_reflns_number_total             2697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02624j2.cif
_cod_data_source_block           rh373
_cod_original_cell_volume        1114.38(14)
_cod_database_code               1552313
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.572
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C9 \\sim C8A-C9A
 with sigma of 0.01
 C8-C10 \\sim C8A-C10A
 with sigma of 0.01
 C10-C11 \\sim C10A-C11A \\sim C11-C12 \\sim C11A-C12A \\sim C13-C14 \\sim
C13A-C14 \\sim C14-C10 ~
 C14A-C10A
 with sigma of 0.01
 C10-C12 \\sim C10A-C12A \\sim C11-C13 \\sim C11A-C13A \\sim C12-C14 \\sim
C12A-C14A \\sim C13-C10 ~
 C13A-C10A \\sim C14-C11 \\sim C14A-C11A
 with sigma of 0.01
 C5-C6 \\sim C5A-C6A
 with sigma of 0.01
 C1-C5 \\sim C1A-C5A \\sim C1-C2 \\sim C1A-C2A \\sim C2-C3 \\sim C2A-C3A \\sim
C3-C4 \\sim C3A-C4A \\sim C4-C5
 \\sim C4A-C5A
 with sigma of 0.01
 C1-C3 \\sim C1A-C3A \\sim C2-C4 \\sim C2A-C4A \\sim C3-C5 \\sim C3A-C5A \\sim
C4-C1 \\sim C4A-C1A \\sim C5-C2
 \\sim C5A-C2A
 with sigma of 0.01
 Ni1-C1 \\sim Ni1A-C1A \\sim Ni1-C2 \\sim Ni1A-C2A \\sim Ni1-C3 \\sim Ni1A-C3A
\\sim Ni1-C4 \\sim Ni1A-C4A
 \\sim Ni1-C5 \\sim Ni1A-C5A \\sim Ni1-C10 \\sim Ni1A-C10A \\sim Ni1-C11 \\sim
Ni1A-C11A \\sim Ni1-C12 ~
 Ni1A-C12A \\sim Ni1-C13 \\sim Ni1A-C13A \\sim Ni1-C14 \\sim Ni1A-C14A
 with sigma of 0.01
 C6-C7 \\sim C6A-C7A
 with sigma of 0.01
 C7-C8 \\sim C7A-C8A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim Ni1 \\sim C1A \\sim C2A
\\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim
C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim Ni1A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=
 Sof(H8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(Ni1A)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(Ni1)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C8A(H8A)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C6A(H6AA,H6AB), C7A(H7AA,H7AB)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C11A(H11A), C12A(H12A), C13A(H13A),
 C14A(H14A)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC)
;
_shelx_res_checksum              37320
_olex2_submission_special_instructions 'No special instructions were received'