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_7131867
_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 N4 O2 Rh, 1.75(C6 H14)'
_chemical_formula_sum            'C80.5 H123.5 Ca2 N4 O2 Rh'
_chemical_formula_weight         1362.40
_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                 97.759(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1756(5)
_cell_length_b                   14.8989(6)
_cell_length_c                   36.7539(13)
_cell_measurement_reflns_used    3686
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.7270
_cell_measurement_theta_min      3.6760
_cell_volume                     7691.4(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.956
_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  0.3167
_diffrn_reflns_av_unetI/netI     0.2896
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            44222
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.131
_diffrn_reflns_theta_min         3.205
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.303
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
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            Orange
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2942
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.781
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00052(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         15187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.2409
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1913
_refine_ls_wR_factor_ref         0.2724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4291
_reflns_number_total             15187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03009a3.cif
_cod_data_source_block           3-Rh
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C80.50 H123.50 Ca2 N4 O2 Rh'
_cod_database_code               7131867
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              64302
_shelx_hkl_checksum              57806
_shelx_fab_checksum              8742