Fe(ii) and Co(ii) N-methylated CYCLEN complexes as paraSHIFT agents with large temperature dependent shifts.
Tsitovich, Pavel B.; Tittiris, Timothy Y.; Cox, Jordan M.; Benedict, Jason B.; Morrow, Janet R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 916–924; doi:10.1039/c7dt03812g

data_7045017
_publ_section_title
;
 Fe(ii) and Co(ii) N-methylated CYCLEN complexes as paraSHIFT agents with
 large temperature dependent shifts.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              916
_journal_page_last               924
_journal_paper_doi               10.1039/c7dt03812g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C22 H34 Co N6, Cl4 Co'
_chemical_formula_sum            'C22 H34 Cl4 Co2 N6'
_chemical_formula_weight         642.21
_chemical_name_systematic        Co(BMPC)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-04 deposited with the CCDC.
2017-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.3640(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8045(5)
_cell_length_b                   12.9067(5)
_cell_length_c                   15.2447(6)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    90
_cell_measurement_theta_max      33.67
_cell_measurement_theta_min      2.19
_cell_volume                     2631.25(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_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 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72080
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.757
_diffrn_reflns_theta_min         1.783
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1066 before and 0.0368 after correction. The Ratio of minimum to maximum transmission is 0.8149. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         10527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0313P)^2^+1.1026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9379
_reflns_number_total             10527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03812g2.cif
_cod_data_source_block           jmc_071403_0m
_cod_depositor_comments          'Adding full bibliography for 7045017.cif.'
_cod_database_code               7045017
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N6(H6), N4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C1(H1a,H1b), C20(H20a,H20b), C10(H10a,H10b), C21(H21a,H21b),
 C8(H8a,H8b), C12(H12a,H12b), C11(H11a,H11b), C19(H19a,H19b), C9(H9a,H9b)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C3(H3), C15(H15), C4(H4a), C5(H5)
2.d Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C18(H18a,H18b,H18c)
;
_shelx_res_checksum              85532
_olex2_submission_special_instructions 'No special instructions were received'