Calcium-Stabilised Transition Metal Bis(Formyl) Complexes: Structure and Bonding
Parr, Joseph; White, Andrew J. P.; Crimmin, Mark Richard; Chemical Communications  (2023) –; doi:10.1039/D3CC03009A

data_7131868
_publ_section_title
;
 Calcium-Stabilised Transition Metal Bis(Formyl) Complexes: Structure and
 Bonding
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03009A
_journal_year                    2023
_chemical_formula_moiety         'C70 H99 Ca2 Ir N4 O2, 1.5(C6 H14)'
_chemical_formula_sum            'C79 H120 Ca2 Ir N4 O2'
_chemical_formula_weight         1430.14
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-05-26 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7586(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2170(3)
_cell_length_b                   14.8985(3)
_cell_length_c                   36.7785(5)
_cell_measurement_reflns_used    5741
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.3690
_cell_measurement_theta_min      4.2940
_cell_volume                     7718.8(2)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            24904
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.472
_diffrn_reflns_theta_min         3.833
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.844
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.585
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         14472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0844P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8974
_reflns_number_total             14472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03009a3.cif
_cod_data_source_block           3-Ir
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7131868
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              37524
_shelx_hkl_checksum              89749
_shelx_fab_checksum              53954